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To cite this Article Singha, A. S. and Thakur, Vijay Kumar(2009)'Chemical Resistance, Mechanical and Physical Properties of
Biofibers-Based Polymer Composites',Polymer-Plastics Technology and Engineering,48:7,736 — 744
To link to this Article: DOI: 10.1080/03602550902824622
URL: http://dx.doi.org/10.1080/03602550902824622
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Polymer-Plastics Technology and Engineering, 48: 736–744, 2009
Copyright # Taylor & Francis Group, LLC
ISSN: 0360-2559 print=1525-6111 online
DOI: 10.1080/03602550902824622
A study on physical and chemical properties along with flame retardancy and corrosion resistance etc. having
mechanical characterization of Hibiscus Sabdariffa fiber-reinforced many industrial applications in various sectors such as
Phenol–Formaldehyde resin matrix based polymer composites have aeronautical, automation, computing, and building
been reported. Effect of fiber dimension on mechanical properties etc.[7,8]. Among phenolics resins phenol–formaldehyde
was evaluated. The interfacial bonding between Hibiscus Sabdariffa
fiber and polymer matrix has been found to affect the properties of based matrix is being used extensively for the production
polymer matrix. It has been observed that particle reinforced poly- of natural fiber reinforced polymer composites as they
mer composites exhibit better mechanical properties as compared to have been found to possess good fiber matrix bonding that
short and long fiber reinforced polymeric composites. These compo- give them better mechanical properties.
sites were further subjected to evaluation of morphological, thermal, It has been observed that lignocellulosic natural fibers
physical (swelling and moisture absorption) and chemical properties.
are able to impart the polymer composite various benefits
such as: low cost, biodegradability, low density; no health
Keywords Mechanical; Morphological and thermal analysis;
Optimization; Polymer composites; Reinforcements hazards; high specific strength, enhanced mechanical
properties, high degree of flexibility, good acoustic and
INTRODUCTION thermal insulation, less machine wear and good availability
etc. as compared to traditional synthetic fibers[9–11].
Present-day industry takes an interest in environment
Perhaps the most attractive characteristic of lignocellulosic
friendly polymer composites materials, due to economic
natural fibers is the clear positive environmental impact
and ecological reasons[1–4]. The use of lignocellulosic
which arises from the fact that these fibers are renewable
natural fibrous materials in composite parts fits well into
and can be easily eliminated at the end of their life
this picture: biofiber which are used as reinforcement to
cycle[12–15]. Therefore, these natural fibers constitute an
reinforce polymer matrices replace synthetic fibers in many
interesting alternative to traditional synthetic fibers in
cases. Clay reinforced by straw was the first known compo-
composite materials. The alternative of natural fibers as a
site material in human history used in building construc-
reinforcing material in polymer composite materials is still
tion developed by the ancient Egyptians approximately
attracting much interest at both the academic and indus-
3,000 years ago. In fact, this composite material was a
trial level. Currently various researchers and material
natural fiber reinforced composite. However, with the
scientists all over the world are focusing their attention
development of materials technology, materials with better
on effective utilization of these natural fibers in polymer
performance, such as ceramics, plastics, metals, and
composites[16,17].
synthetic fibers composites were intensively used and the
The commercial importance of polymers have derived
use of natural fiber composite was discarded for very
intense applications in the form of composites in various
long time. Recently, the use of lignocellulosic natural
fields such as in automotive, aerospace, marine, infrastruc-
fiber-reinforced polymer composites has started gaining
ture etc. In spite of a number of advantages the natural
attractiveness in engineering applications[5,6].
fiber reinforced composites have few disadvantages also.
Among various polymer matrices, phenolics resins are
One of the serious problems related to the use of lignocel-
known as the oldest and one of widely used thermosetting
lulosic fibers and fabrics in polymer composites materials is
polymers because of its low cost, high mechanical
their affinity towards moisture. Indeed the potential use of
natural fibers as a reinforcement of polymer matrices is
Address correspondence to A. S. Singha, Applied Chemistry
Research Laboratory, National Institute of Technology greatly harmed by their hydrophilic character, high capa-
Hamirpur 177005, Himachal Pradesh, India. E-mail: assingha@ city of moisture absorption and poor adhesion between
gmail.com them and the matrix[18–20].
736
BIOFIBERS-BASED POLYMER COMPOSITES 737
Natural fibers like flax, jute, pinus, saccaharum cilliare by weight, in the reaction kettle and were mixed with the
fiber, oil palm are frequently being used as reinforcing help of mechanical stirrer. Suitable conditions of tempera-
material in a number of applications. Among various types ture, acidity of the medium and pH were maintained while
of natural fibrous material, Hibiscus Sabdariffa has high carrying out the reaction as reported earlier[8]. The resin
potential as a reinforcing material in polymer composites. synthesized was then transferred to a specially made mold.
Literature review has revealed that a very little work has Resin sheets of size 150 mm 150 mm 5.0 mm were
been done on the use of Hibiscus Sabdariffa as reinforcing prepared by a closed mold method[6–11]. The cured samples
material in the polymer composites[21–25]. In the present were then subjected to various mechanical, thermal and
manuscript we have reported our studies on the synthesis morphological studies.
of Phenol–Formaldehyde (PF) resin matrix based polymer
composites and evaluation of their mechanical morphologi- Synthesis of Polymer Composites
cal and thermal properties. A study on the swelling Particle Reinforced Composites. Hibiscus Sabdariffa
behaviour, moisture absorbance and chemical resistance fibers were grinded to a powder and filtered through a sieve
behaviour of polymer matrix and fiber-reinforced polymer of pore size 200 microns. The specific amount of Phenol–
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composites under different intervals of time has also been Formaldehyde (PF) resin and Hibiscus Sabdariffa fibers
reported. were taken and mixed thoroughly by suitable loading (1:
0.1). The above mixture was poured into a specially made
EXPERIMENTAL mold. The surfaces of molds were coated on the inside with
Materials and Methods oleic acid to avoid adhesion of the mixture and to allow
Phenol, formaldehyde solution and sodium hydroxide easy removal of the composites. The mixture was then
supplied by Qualigens Chemicals Ltd Company were used spread equally on the surface of the mold. Composite
as received. In the present research work we have used sheets of size 150 mm 150 mm 5.0 mm were prepared
phenolics resin such as Phenol–Formaldehyde (PF) as poly- by compression molding technique on Compression Mold-
mer matrix and lignocellulosic natural fibers as reinforcing ing Machine. Compression molding was performed in a
material. Hibiscus Sabdariffa fibers collected from local hot press using a mold preheated to 120 C. The material
resources were used as natural fibrous material as the first placed in a hot open mold was left for about 5 min,
reinforcement in the polymer composite. The fibers prior and then the mold was closed. Composite sheets were
to use were washed thoroughly with detergent powder prepared by hot pressing the mold at 150 C for 30 min at
because fibers generally contain some impurities that may a pressure of 4 MPa. The specimens were then post cured
affect the bonding between the fibers and the polymer at 120 C for 12 hr and were subjected for different mechan-
matrix. After this these fibers were washed with distilled ical and thermal studies.
water and dried in an air oven at 70 C for 12 h and a Short-Fiber Reinforced Composites. Hibiscus Sabdar-
vacuum oven at 67 C for 3 h before preparation of com- iffa fibers were cut into 3 mm size and mixed with the
posites. These fibers were used in three forms: 1. Particle weighed amount of Phenol–Formaldehyde (PF). Composite
Reinforcement (200 m); 2. Short-Fiber Reinforcement sheets were prepared as per method discussed above.
(3 mm); and 3. Long Fiber Reinforcement (6 mm).
Long-Fiber Reinforced Composites. Hibiscus Sabdar-
iffa fibers were cut into 6 mm length and mixed with
Instruments Used
weighed amount of resin. Curing of samples was done as
Weights of the samples were taken on Shimadzu make
per the method discussed earlier.
electronic balance (LIBROR AEG-220), curing of samples
was done on compression molding machine (SANTECH Mechanical Analysis of Resin and Polymer
INDIA Ltd), thermal studies were carried out on Thermal Composite Samples
Analyzer (Perkin-Elmer) and SEM micrographs were taken
Tensile Strength Test. The tensile strength test was
on (LEO 435VP). Tensile, compressive and flexural strength
conducted on Computerized Universal Testing Machine
tests were performed on Computerized Universal Testing
(HOUNSFIELD H25KS). The sample of 10 cm length
Machine (HOUNSFIELD H25KS). Wear test was per-
was clamped into the 2 jaws of the machine. Each end of
formed on Wear & Friction Monitor (DUCOM-TR-20L).
the jaws covered 2 cm of the sample. Tensile strength was
studied over the rest of 6 cm gauze length. Reading of the
Synthesis of Phenol–Formaldehyde Resin tensile strength test instrument for Newton force and
Phenol–Formaldehyde resin has been synthesized by the extension was initially set at zero. The test was conducted
standard method developed in our material science labora- at the constant strain rate of the order of 10 mm=min.
tory[8,15]. Phenol and formaldehyde were taken in different Tensile stress was applied till the failure of the sample
molar ratio (1.0:1.0, 1.0:1.5, 1.0:2.0, 1.0:2.5, and 1.0:3.0) and load – extension curve was obtained.
738 A. S. SINGHA AND V. K. THAKUR
Compressive Strength Test. Compression strength of change upon heating versus temperature is plotted and
samples was also tested on Computerized Universal Testing is used to simplify reading of weight-versus temperature
Machine (HOUNSFIELD H25KS). Composite sample was thermogram peaks that occur close together. DTG peaks
held between the two platforms and the strain rate was fixed are characterized by the peak maximum (Tmax) and the
at 10 mm=min, whereas the total compression range was peak on set temperature (Te). The area under DTG curve
7.5 mm. The compression stress was applied till the failure is proportional to the mass change and the height of the
of sample. Total compression per unit force was noted. peak at any temperature gives the rate of the mass change
at that temperature. DTG curves are frequently preferred
Flexural Strength Test. Flexural strength of samples when comparing results with DTA curves because of the
was also tested on Computerized Universal Testing visual similarity.
Machine. The three-point bend flexural test was conducted
in accordance with ASTM D 790 method. Chemical Resistance, Swelling, and Moisture
Wear Test. The wear test of the testing sample was Absorbance Behaviour
The effect of environmental conditions on the polymer
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Wf Wi
% Moisture absorbance ð% Mabs Þ ¼ 100
Wi
wear resistance etc.[6,10]. It has been observed that Phenol– iii. Long-fiber reinforced composite could bear a load of
formaldehyde resin in the ratio 1:1.5 exhibit optimum 1247.0 N at an extension of 3.1 mm.
mechanical properties so this ratio was taken for further
Compressive Strength. Compressive strength of PF
fabrication of polymer composites. The wear resistance
resin matrix has been found to increase when reinforced
results also supports the tensile, compressive and flexural
with Hibiscus Sabdariffa. It has been found that with par-
results, as brittle materials have higher wear rate and low
ticle reinforcement, compressive strength increases to a
tensile, compressive and flexural strength. The ratio
much more extent than short and long fiber reinforcement
(1.0:1.5) of Phenol and formaldehyde showing optimum
(Figure 2B). It is clear that the samples of
mechanical properties was taken for further preparation of
biomass reinforced Phenol–formaldehyde biocomposites. i. Particle-reinforced composite could bear a load of
3535.5 N with compression of 2.68 mm.
Mechanical Properties of PF Matrix-Based ii. Short-fiber reinforced composite could bear a load of
Polymer Composites 3387.8 N with compression of 2.75 mm.
Tensile Strength. It has been observed that polymer iii. Long-fiber reinforced composite could bear a load of
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composites with particle reinforcement showed more 3302.4 N with compression of 2.79 mm.
tensile strength which was followed by short fiber and long
Flexural Strength. Flexural strength of PF resin
fiber reinforced composites (Figure 2A). It is clear from the
matrix has been found to follow the same trend as is
(Figure 2A) that the samples of
observed for tensile and compressive strength. It has been
i. Particle-reinforced composite could bear a load of found that with particle reinforcement, compressive
1325.0 N at an extension of 2.94 mm. strength increases to a much greater extent than short-
ii. Short-fiber reinforced composite could bear a load of and long-fiber reinforcement (Figure 2C). It is clear that
1275.0 N at an extension of 3.03 mm. the samples of
FIG. 2. Load elongation=deformation=deflection and wear resistance curve of fiber-reinforced composites (A, B, C, and D).
BIOFIBERS-BASED POLYMER COMPOSITES 741
i. Particle-reinforced composite could bear a load of within the macromolecule itself, along with hydroxyl groups
1037.0 N with compression of 2.63 mm. of Phenolic (Phenol–Formaldehyde) resin. It can be
ii. Short-fiber reinforced composite could bear a load of concluded that different degrees of reinforcement effects
980.0 N with compression of 2.69 mm. are achieved by the addition of Hibiscus Sabdariffa fibers
iii. Long-fiber reinforced composite could bear a load of to Phenol–Formaldehyde (PF) resin matrix-based polymer
940.0 N with compression of 2.72 mm. composites. This property also leads to increase in mechan-
ical properties of the Hibiscus Sabdariffa fiber-reinforced
Wear Test. As evident from (Figure 2D) wear rate of polymer composites.
PF matrix decreases appreciably when it is reinforced with
Hibiscus Sabdariffa. It was observed that particle reinforce- Morphological Study of Polymer Biocomposites
ment decreases the wear rate to a much greater extent than Morphological results (Figure 3) show that there is
short and long fiber reinforcement. From these results it is proper intimate mixing of Hibiscus Sabdariffa fibers with
clear that particle reinforcement is more effective than short- the Phenol–Formaldehyde (PF) resin matrix in the polymer
and long-fiber reinforcement. This may be due to larger composites thus synthesized. Morphological results
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surface area and more fiber=matrix interaction in case of evidently demonstrate that when polymer resin matrix is
particle-reinforced composites. Further the interfacial bond- reinforced with the different dimension of fiber, morpholo-
ing between polymer matrix and lignocellulosic biofiber gical changes take place depending upon the interfacial
depends on the surface topology of these natural fibers[6–10]. interaction between the varying loading of fiber and the
The interface acts as a ‘binder’ and transfers load between resin matrix[6–10].
the matrix and the reinforcing fibers. The interfacial area
plays a major role in determining the strength of polymer Thermal Behaviour of Polymer Resin and its Composites
composite material because each fiber forms an individual Thermogravimetric analysis (TGA) of raw Hibiscus
interface with the matrix. In lignocellulosic natural fibers Sabdariffa fiber, polymeric Phenol–Formaldehyde (PF)
cellulose is the major component containing strong hydroxyl resin and biocomposites was studied as a function of %
groups in its structure which tend to form hydrogen bonds weight loss with the increase in temperature. For Hibiscus
FIG. 3. SEM images of (A) Phenol–Formaldehyde resin (B, C, & D) composite with particle, short and long fiber reinforcements.
742 A. S. SINGHA AND V. K. THAKUR
TABLE 1
TGA=DTA analysis of PF, HS and P-Rnf-PF Composites
Sr. Sample IDT % FDT % Final Exothermic=endothermic
No. code ( C) wt. loss ( C) wt. loss residue (%) peaks C(mV)
1. HS 199 7.65 500 85.71 14.29 63[0.9]; 361[1.5]
2. PF Resin 400 15.68 1195 48.53 51.47 164[9.0]; 421[6.0]
3. P-Rnf Comp 332 25.39 981 57.25 42.75 63[2]; 687[27]
TABLE 5
Moisture absorption (in terms of %) behavior of polymer composites at different relative humidity levels
% Loading Hum ¼ 20 Hum ¼ 40 Hum ¼ 60 Hum ¼ 80 Hum ¼ 100
PF Resin 0.00009 0.00018 0.00027 0.00043 0.00058
P-Rnf 0.00014 0.00025 0.00039 0.00055 0.00066
SF-Rnf 0.00018 0.00029 0.00045 0.00061 0.00072
LF-Rnf 0.00024 0.00035 0.00049 0.00067 0.00078
(Mabs) increases with increase in humidity level ranging 3. Naik, J.B.; Mishra, S. Esterification effect of maleic anhydride on
from 20 to 100%. surface and volume resistivity of natural fiber=polystyrene composites.
Polym. Plast. Technol. Eng. 2007, 46 (5), 537–540.
4. Bledzki, A.K.; Faruk, O. Wood fiber reinforced polypropylene
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glass-bamboo-bisphenol-C-formaldehyde-acrylate a value added com- 22. Singha, A.S.; Thakur, V.K. Mechanical, thermal and morphological
posites. Polym. Plast. Technol. Eng. 2007, 46 (6), 621–628. properties of G. Optiva fiber=polymer matrix composites. Polymer
20. Kumar, S.M.N. Siddaramaiah Studies on acrylonitrile-butadiene Plastic Technol. Eng. 2009, 48 (2), 201–208.
(NBR) latex-reinforced jute nonwoven fabric composites: Chemical 23. Singha, A.S.; Thakur, V.K. Saccaharum Cilliare fiber reinforced
resistance, mechanical properties, and water absorption. Polym. Plast. polymer composites. E-J. Chem. 2008, 5, 782–791.
Technol. Eng. 2006, 45 (3), 409–414. 24. Bhatnagar, A.; Sain, M. Processing of cellulose nanofiber-reinforced
21. Singha, A.S.; Thakur, V.K. Evaluation of mechanical properties of composites. J. Reinf. Plasti. Compos. 2005, 24, 1259–1268.
natural fiber reinforced polymer composites. Inter. J. Plast. Technol. 25. Bledzki, A.K.; Gassan, J. Composites reinforced with cellulose based
2008, 12, 913–923. fibers. Prog. Polym. Sci. 1999, 24, 221–274.
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