Bull. Mater. Sci., Vol. 32, No. 1, February 2009, pp. 49–58. © Indian Academy of Sciences.

Fabrication and characterization of S. cilliare fibre reinforced polymer

composites

A S SINGHA* and VIJAY KUMAR THAKUR

Department of Chemistry, National Institute of Technology, Hamirpur 177 005, India

MS received 16 March 2008

Abstract. In the recent times, there has been an ever-increasing interest in green composite materials for its
applications in the field of industries, aerospace, sports, household etc and in many other fields. In this paper,
fabrication of Saccharum cilliare fibre reinforced green polymer composites using resorcinol formaldehyde
(RF) as a novel matrix has been reported. A systematic approach for processing of polymer is presented.
Effect of fibre loading on mechanical properties like flexural, tensile, compressive and wear resistances has
also been determined. Reinforcing of the RF resin with Saccharum cilliare (SC) fibre was done in the form of
particle size (200 micron). Present work reveals that mechanical properties of the RF resin have been found to
increase up to 30% fibre loading and then decreases. Morphological and thermal studies of the resin, fibre
and particle reinforced (P-Rnf) green composites have also been studied.

Keywords. Composites; reinforcements; optimization; mechanical properties.

1. Introduction etc have become important considerations in the fabrica-

tion of new products (Hagstrand and Oksman 2001; Kaith
Over the past few decades, polymers have replaced many et al 2005, 2007; Singha and Shama 2007a). At present
of the conventional materials in a variety of applications. various workers are focusing their attention on use of
This is possible because of the advantages polymers offer natural fibres in place of synthetic fibres in various fields
over conventional materials. Ease of processing, producti- especially as reinforcing fillers (Nabi Saheb and Jog
vity, and decrease in cost of the materials are the most 1999; Nakagiato and Yano 2004; Singha et al 2005; Pan-
important advantages of using polymers in a number of thapulakkal et al 2006; Kaith et al 2008). Natural fibre
fields. Emerging community concerns and a growing reinforced polymer composites have recently been pre-
environmental awareness throughout the world has forced ferred over composites prepared with ceramic and metal
the researchers to synthesize new green materials and matrix because of their better properties. Natural fibre-
processes that enhance the environmental quality of pro- reinforced polymers offer advantages over other conven-
ducts (Chauhan et al 2000a,b; Bhatnagar and Sain 2005; tional materials when specific properties are compared.
Singha et al 2008a,b). In most of its applications, the These composites are finding applications in diverse fields
properties of polymers are modified using natural fillers from appliances to spacecrafts. The use of natural fibres
and natural fibres to suit the high strength/high modulus derived from a number of renewable resources as rein-
requirements (Bledzki et al 1996, 1998; Bledzki and Gas- forcing fibres in both thermoplastic and thermoset matrix
son 1999; Chauhan et al 1999, 2001; Singha et al 2002). composites provides positive environmental benefits and
Keeping in view the eco-friendly advantages of green offer numerous advantages over conventional materials
materials a large number of industries throughout the world including lightness, resistance to corrosion, abrasion and
are initiating the design and engineering of these pro- ease of processing etc (Gassan and Bledzki 1997; Velde
ducts. Sustainable growth and eco-efficiency are of most van de and Kiekens 2001, 2003; Kaith et al 2008). Natu-
importance to the majority of industries. At present greater ral fibres like flax, jute, pinus, Saccharum cilliare oil
attention is being given for the production of green com- palm have all been proved to be good reinforcements in
posites which can help in resolving future environmental thermoset and thermoplastic matrices. Saccharum cilliare
problems (Gatenholm et al 1993; Gassan and Bledzki fibre is abundantly found in Himachal Pradesh. The lit-
1997; De and Adhikari 2004). In this perspective easy erature survey has revealed that no work has been done
availability, biodegradability, eco-friendliness, light weight on utilization of this fibre as reinforcing material in the
polymer composites (Singha et al 2008a, b). Keeping in
view the easy availability and many other ecofriendly
*Author for correspondence ([email protected]) advantages, we have used this fibre as reinforcing mate-

49
50 A S Singha and Vijay Kumar Thakur

rial for the preparation of resorcinol-formaldehyde (R-F) 30 and 40%) in terms of weight. The surfaces of molds to
resin based green composites. The green composites so be used were coated on the inside with oleic acid to avoid
prepared were subjected to evaluation of their mechanical, adhesion of the mixture and to allow easy removal of the
morphological and thermal properties. composites. The above mixture was poured into a spe-
cially made mold. The mixture was then spread equally
on the surface of the mold. Composite sheets of size
2. Experimental
150 × 150 × 5⋅0 mm were prepared by compression mold-
ing technique on a Compression Molding Machine. Com-
2.1 Materials
pression molding was performed in a hot press using a
mold preheated to 50°C. The material first placed in a hot
Resorcinol and formaldehyde solutions were supplied by
open mold was left for about 5 min, and then the mold
Qualigens Chemicals Ltd and were used as received.
was closed. Composite sheets were prepared by hot press-
Resorcinol–formaldehyde (R–F) was used as a matrix
ing the mold at 50°C for 30 min. The pressure applied
polymer. The natural fibrous materials used as the rein-
ranges from 3–4 MPa depending on the loading of rein-
forcing filler in the composite were Saccharum cilliare
forcing material. All the specimens were then post cured
fibres of particle dimensions (200 μm). Weights of the
at 50°C for 12 h.
samples were taken on Shimadzu make electronic balance
(LIBROR AEG-220), curing of samples was done on
compression molding machine (SANTECH INDIA Ltd), 2.4 Mechanical testing
thermal studies were carried out on thermal analyser
(Perkin Elmer) and SEM micrographs were taken on LEO Tensile, compressive, flexural and wear tests were per-
435VP. formed on specimens cut from the above prepared com-
posite material. Seven specimens of each sample were
2.2 Synthesis of resorcinol–formaldehyde resin used for the determination of mechanical properties and
the tests were conducted at ambient laboratory environ-
Resorcinol–formaldehyde (RF) resin was synthesized by ment. Testing of samples for tensile, compressive and
the standard method developed in our Applied Chemistry, flexural strengths were done on Computerized Universal
Research Laboratory (Singha and Thakur 2007b). Resor- Testing Machine (HOUNSFIELD H25KS), wear testing
cinol and formaldehyde were taken in different molar was done on Wear & Friction Monitor (DUCOM-TR-20L).
ratios (1⋅0 : 1⋅0, 1⋅0 : 1⋅5, 1⋅0 : 2⋅0, 1⋅0 : 1⋅5 and 1⋅0 : 3⋅0) by
weight, in a reaction kettle and were mixed with the help 2.5 Analysis of mechanical properties of samples
of a mechanical stirrer. Since the reaction is exothermic,
proper care was taken to maintain the temperature bet- The tensile strength test was conducted on Computerized
ween 40 and 45°C, for initial 1 h. Then temperature was Universal Testing Machine (HOUNSFIELD H25KS). The
increased to 50°C and the mixture was heated at this tempe- specimens of dimension 100 × 10 × 5 mm were used for
rature, till complete resinification. Then heating was analysis. The tensile test was conducted in accordance
stopped and the resin was cooled. The resin synthesized with ASTM D 3039 method. The test was conducted at a
was then transferred to a specially made mould. Resin constant strain rate of 10 mm/min. Force was applied till
sheets of size 150 × 150 × 5⋅0 mm were prepared by a the failure of the sample and load-elongation curve was
closed mould method as described somewhere else (Sin- obtained. The compression test was conducted in accor-
gha et al 2005). The mould was then closed and kept dance with ASTM D 3410 method. Composite sample
under pressure (4⋅0 MPa) until the resin was set into a hard was held between the two platforms and the strain rate
mass. All the specimens were post cured at 55°C for 5 h. was fixed at 10 mm/min whereas the total compression
range was 7⋅5 mm. The compression stress was applied
2.3 Synthesis of polymer biocomposites till the failure of sample. Flexural strength of samples
was also tested on Computerized Universal Testing
Saccharum cilliare fibres collected were first thoroughly Machine. The three-point bend flexural test was conducted
washed with detergent powder. After this these were in accordance with ASTM D 790 method. The wear test
soaked in hot distilled water for 3 h, dried for 48 h in air of the sample was conducted on Wear & Friction Monitor
at room temperature followed by drying at 100°C for 24 h (DUCOM-TR-20L). Wear resistance of composites was
to adjust it to a moisture content of 1–2% and then stored carried out as per ASTM D 3702 method.
over desiccant in sealed container. The dried Saccharum
cilliare fibres were grinded to a powder of pore size 2.6 SEM analysis of samples
200 μm. Thorough mixing of Saccharum cilliare fibre
particles with resorcinol–formaldehyde resin was done In order to evaluate changes in the composite surface
using mechanical stirrer with different loadings (10, 20, morphology, fibres and matrix were analysed by scanning
 Fabrication and characterization of S. cilliare polymer composites 51

electron microscopy (SEM). The excitation energy used Reaction between formaldehyde and resorcinol proceeds
was 5 keV. To achieve good electric conductivity all sam- vigorously towards thermosetting state when these are
ples were first carbon sputtered followed by sputtering a heated together. Hence proper care must be taken while
gold palladium mixture before examination. SEM micro- carrying out the reaction. Methylolated resorcinols con-
graphs of the samples show the morphology of the poly- dense with formaldehyde molecules and other resorcinol
mer composites prepared. These micrographs clearly show molecules to form polymeric structure as shown in scheme
the difference between unloaded and loaded RF matrix. 2. In these reactions resorcinol nuclei are joined together
through methylene bridges to give complex molecule.
Complete methylene bridging is shown in scheme 3.
2.7 Thermal analysis of samples

Thermal analysis of natural and synthetic polymers gives 3.2 Optimization of resorcinol–formaldehyde resin
us good account of thermal stability of materials. Thermo-
gravimetric analysis (TGA) and differential thermal Optimization of resorcinol–formaldehyde resin was done
analysis (DTA) studies of samples were carried out in by taking the mechanical properties such as tensile strength,
nitrogen atmosphere on a thermal analyser (Perkin Elmer) compressive strength, flexural strength and wear resi-
at a heating rate of 10°C/min. TGA is used to characte- stance into consideration.
rize the decomposition and thermal stability of materials
under a variety of conditions, and to examine the kinetics 3.2a Tensile strength: It has been observed that RF
of the physico-chemical processes occurring in the sam- samples of ratio 1⋅0 : 1⋅5 bear more load at a particular
ple. Basically in this method a change in thermal stability applied load as compared to samples of other ratios (Singha
is examined in terms of percentage weight loss as a func- and Thakur 2007b). This ratio (1⋅0 : 1⋅5) could bear a load
tion of temperature. The mass change characteristics of a of 250⋅8 N with an extension of 2 mm (figure 1). On the
material are strongly dependent on the experimental con- other hand, samples of other ratios bear low loads.
ditions such as sample mass, volume and physical form,
the shape and nature of the sample holder, the nature and 3.2b Compressive strength: It is evident from figure 2
pressure of the atmosphere in the sample chamber and the that the samples of ratio 1⋅0 : 1⋅5 could bear a load of
scanning rate and all have important influences on the 1370 N at a compression of 2⋅17 mm.
characteristics of the recorded TG curve. At the same
time DTA involves comparing the precise temperature 3.2c Flexural test: It is evident from figure 3 that the
difference between a sample and an inert reference mate- samples of ratio 1⋅0 : 1⋅5 could bear a maximum load of
rial, while heating both. 117⋅8 N at a deflection of 1⋅0 mm.

3. Results and discussion

In the study of the behaviour of polymer composites,

mechanical analysis is a tool of chief importance. It has
been proved to be an efficient method to study the beha-
Scheme 1. Formation of methylol derivative.
viour of the materials under different conditions of tension,
compression, stress–strain and its role in determining the
mechanical properties. Generally mechanical properties
of fibre reinforced composites depend on the nature of
the matrix material, the distribution and orientation of the
reinforcing material and the content of the fibre loading.

3.1 Mechanism of synthesis of resorcinol–

formaldehyde resin Scheme 2. Condensation reaction of methylated resorcinol to
form polymeric structure.
Resorcinol is a very reactive compound and readily com-
bines with formaldehyde to form methylene derivative
(Pizzi and Cameron 1989). In this reaction methylol
group occupies either the position ortho to both hydroxyl
groups or ortho to one and para to other as shown in
scheme 1. The reaction is carried out in neutral medium Scheme 3. Methylene bridging in polymerized resorcinol
as resorcinol is very reactive towards formaldehyde. molecules.
52 A S Singha and Vijay Kumar Thakur

3.2d Wear resistance: It has been observed that wear The wear resistance results also support the tensile,
rate of samples of ratio 1⋅0 : 1⋅5 was less as compared to compressive and flexural results, as brittle materials have
any other samples. Loss of material was due to abrasion higher wear rate and low tensile, compressive and fle-
and friction of samples with disc (figure 4). xural strength. The ratio (1⋅0 : 1⋅5) of resorcinol and for-

Figure 4. Wear resistance of RF resin.

Figure 1. Load-elongation curve of RF resin.

Figure 5. Load-elongation curve of P-Rnf composite with

different loadings.
Figure 2. Load-deformation curve of RF resin.

Figure 6. Load-deformation curve of P-Rnf composite with

Figure 3. Load-deflection curve of RF resin. different loadings.
 Fabrication and characterization of S. cilliare polymer composites 53

maldehyde showing optimum mechanical properties was 3.3 Effect of reinforcement on mechanical properties of
taken for further preparation of biomass reinforced resor- RF matrix based polymer composites
cinol–formaldehyde biocomposites.
3.3a Tensile strength: It has been observed that tensile
strength of composites increases on reinforcement with
Saccharum cilliare fibre. Composites with 30% wt. load-
ing bear maximum load followed by 40%, 20%, and 10%
loadings (figure 5). It has been observed that polymer
composite with 30, 40, 20 and 10% loading bear a load of
755⋅37 N, 685⋅00 N, 570⋅00 N and 481⋅58 N, respectively.

3.3b Compressive strength: Compressive strength of

RF matrix has been found to increase as reinforcement
with Saccharum cilliare needles. It has been found
that on particle reinforcement compressive strength
increases to a much more extent. The compressive pro-
perties of the composites as a function of load and defor-
mation are presented in figure 6. From the graph it is
evident that first compressive force increases with the
increase in fibre content but after 30% fibre content a
Figure 7. Load-deflection curve of P-Rnf composite with significant decrease in compressive strength is observed.
different loadings.

Figure 8. Wear resistance of P-Rnf composite with different Figure 10. Compressive stress–strain curve of P-Rnf composite.
loadings.

Figure 9. Tensile stress–strain curve of P-Rnf composite. Figure 11. Flexural stress–strain curve of P-Rnf composite.
54 A S Singha and Vijay Kumar Thakur

Table 1. Values of various parameters obtained from tensile stress–strain curve at different loadings.
Fibre loading Ultimate tensile stress Yield strength Fracture stress Standard Tensile modulus
(wt. %) (N/mm2) (N/mm2) (N/mm2) deviation (N/mm2)

10% 9⋅63 8⋅07 9⋅01 1⋅54 251⋅02

20% 11⋅40 9⋅08 10⋅74 1⋅75 301⋅70
30% 15⋅57 12⋅69 14⋅38 1⋅96 419⋅28
40% 13⋅87 11⋅84 12⋅79 2⋅01 387⋅48

perties of samples as a function of force (in terms of load)

and deflection are shown in figure 7. It is clear from the
figure that composite with 30, 40, 20 and 10% loading
bear a load of 345⋅32 N, 291⋅00 N, 250⋅00 N and
181⋅64 N, respectively.

3.3d Wear test: As evident from figure 8, wear rate

of RF matrix decreases appreciably as reinforcement with
Saccharum cilliare fibre. It was observed that particle
reinforcement decreases the wear rate to a much more
extent. Maximum wear resistance behaviour is shown by
composite with 30% loading followed by 40, 20 and 10%
loading.

3.3e Stress–strain behaviour: (i) Tensile stress–strain

curve: Tensile stress–strain curve is constructed from
the load elongation measurements. Tensile stress is obtained
on dividing the load by the original area of the cross sec-
Figure 12. SEM of RF resin.
tion of the specimen. The strain used for the compressive
stress–strain curve is the average linear strain, which is
obtained on dividing the elongation of the gauge length
of the specimen, by its original length. Since both stress
and strain are obtained by dividing the load and elonga-
tion by constant factors, the stress–strain curve has the
same shape as the load-elongation curve. The plot
of stress vs strain for Saccharum cilliare fibre rein-
forced polymer composites is shown in figure 9. From the
figure it is clear that in the elastic region stress is linearly
proportional to strain. When the load exceeds a value
corresponding to the yield strength, the specimen under-
goes gross plastic deformation. It is permanently deformed
if the load is released to zero. Different parameters
derived from the tensile stress–strain curve are shown in
table 1.

(ii) Compressive stress–strain curve: Compressive

stress–strain curve is constructed from the load deforma-
Figure 13. SEM of raw Saccharum cilliare fibre. tion measurements. Compressive stress is obtained on
dividing the load by the original area of the cross section
It is clear from the figure that composite with 30, 40, of the specimen. The strain used for the compressive
20 and10% loading bear a load of 4247⋅8 N, 3860⋅7 N, stress–strain curve is the average linear strain, which is
3293⋅7 and 2496⋅5 N, respectively. obtained on dividing the deformation of the gauge
length of the specimen, by its original length. The
3.3c Flexural strength: Similar trends as obtained in compressive stress–strain curve has the same shape as
tensile strength and compressive strength tests have been the load-deformation curve. The plot of compressive
observed for flexural strength results. The flexural pro- stress vs strain for Saccharum cilliare fibre reinforced
 Fabrication and characterization of S. cilliare polymer composites 55

Table 2. Values of various parameters obtained from compressive stress–strain curve at different loadings.
Fibre loading Ultimate compressive Yield strength Fracture stress Standard Compressive
(wt. %) stress (N/mm2) (N/mm2) (N/mm2) deviation modulus (N/mm2)

10% 49⋅93 40⋅66 46⋅7 1⋅95 1323⋅70

20% 65⋅87 55⋅42 61⋅78 1⋅99 1757⋅00
30% 84⋅94 72⋅26 77⋅37 2⋅15 2277⋅00
40% 77⋅20 66⋅36 73⋅42 2⋅31 2069⋅00

Table 3. Values of various parameters from flexural stress–strain curve for different percentage of loading.
Fibre loading Ultimate flexural stress Yield strength Fracture stress Standard Flexural modulus
(wt. %) (N/mm2) (N/mm2) (N/mm2) deviation (N/mm2)

10% 54⋅49 41⋅56 48⋅47 1⋅47 3338⋅97

20% 75⋅00 63⋅14 69⋅02 1⋅83 4044⋅11
30% 103⋅59 94⋅73 99⋅85 1⋅94 5979⋅77
40% 87⋅30 79⋅07 84⋅97 1⋅89 4981⋅61

The plot of flexural stress vs strain for Saccharum cilliare

fibre reinforced polymer composites is shown in figure
11. Different parameters derived from the tensile stress–
strain curve are shown in table 3.
In order to achieve good fibre reinforcement, interfacial
strength between the fibre and matrix is the most essen-
tial factor. For a composite to be an effective load bearing
system, the fibres and matrix must cooperate. This coop-
eration between the fibres and the matrix will not exist
without the presence of the interface. The interfacial
strength depends on the surface topology of the fibre. The
interface acts as a ‘binder’ and transfers load between the
matrix and the reinforcing fibres. The interfacial area
plays a major role in determining the strength of composite
material because each fibre forms an individual interface
with the matrix. Interfacial bonding is a result of good
wetting of the fibres by the RF matrix as well as the for-
Figure 14. SEM of composite with 10% fibre loading.
mation of a chemical bond between the fibre surface and
the RF matrix. Hence the interface plays a key role in
polymer composites is shown in figure 10. From the fig- controlling the mechanical properties of a composite. It
ure it is clear that in the elastic region stress is linearly can be concluded that different degrees of reinforcement
proportional to strain. When the load exceeds a value effects are achieved by the addition of natural fibres to
corresponding to the yield strength, the specimen under- RF matrix based polymer. This may be due to the differ-
goes gross plastic deformation. It is permanently ent adhesion strengths between matrices and fibres. The
deformed if the load is released to zero. Different para- adhesion is usually the strongest in polar polymers capable
meters derived from the tensile stress–strain curve are of forming hydrogen bonds with hydroxyl groups avai-
shown in table 2. lable on the fibre surface. The chemical bonding accounts
for the adhesion between RF resin and cellulose of fibre.
(iii) Flexural stress–strain curve: Flexural stress– Still higher bond strength obtained for RF resin matrix is
strain curve is also constructed from the load deformation due to the possible reaction between the methylol groups
measurements. Flexural stress is obtained by dividing the of the resin with the hydroxyl group of cellulose.
load by the original area of the cross section of the Supplementary after a certain higher fibre loading a
specimen. The strain used for the flexural stress–strain decrease in the mechanical properties of RF matrix based
curve is the average linear strain, which is obtained by composites is observed. It has been observed that mechani-
dividing the deflection of the gauge length of the speci- cal properties increase up to 30% fibre loading and then
men, by its original length. The flexural stress–strain decreases. The mechanical strength of RF composites
curve has also the same shape as the load-deflection curve. levels off at high fibre loading. This behaviour can be
56 A S Singha and Vijay Kumar Thakur

explained due to fibre–fibre contact at higher fibre load- ing in the case of random orientation. At higher levels of
ing. Hence lower results are obtained for 40% loading. fibre loading, the increased population of fibres led to
Further when fibre-reinforced RF composites were sub- agglomeration, and stress transfer was partially blocked
jected to a load, the fibres acted as carriers of load, and resulting in lowering of mechanical properties after 30%
stress was transferred from the matrix along the fibres loading.
which resulted in composites with good mechanical pro- These results suggest that Saccharum cilliare fibre has
perties. The uniform distribution of stress was dependent immense scope in the fabrication of natural fibre rein-
on the population and orientation of the fibres. At low forced polymer composites having vast number of indus-
levels of fibre loading, the orientation of fibres was poor, trial applications. Further this can provide employment to
the fibres were not capable of transferring load to one a number of villagers.
another, and stress accumulated at certain points of the
composite, which led to a lower mechanical properties.
3.4 Morphological study of biocomposites
At 30% levels of loading the population of the fibres is
just right for maximum orientation and the fibres actively
Morphological results (figures 12–17) show that there is
participate in stress transfer and hence maximum results
proper intimate mixing of fibre with the resin in the bio-
are obtained in case of this loading. As discussed, modulus
composites thus synthesized. Morphological results evi-
showed a clear continuous increase up to 30% fibre load-
dently demonstrate that when polymer resin matrix is
reinforced with different loadings of fibre, morphological
changes take place depending upon the interfacial inter-
action between the varying loading of fibre and the resin
matrix.

3.5 Thermal behaviour of RF resin and its composites

Thermogravimetric analysis (TGA) of raw fibre, poly-

meric resin and biocomposite with 10% loading was stud-
ied as a function of % weight loss with the increase in
temperature. In case of raw fibre, in the beginning of
depolymerization, dehydration and glucosan formation
took place between the temperature ranges of 26⋅0°C and
195⋅0°C followed by the cleavage of C–H, C–C and C–O
bonds. Initial decomposition (IDT) temperature is 212°C
and final decomposition temperature is 471°C. On the
other hand, in case of polymeric resin (resorcinol formal-
dehyde), it is single stage decomposition and the initial
Figure 15. SEM of composite with 20% fibre loading.

Figure 16. SEM of composite with 30% fibre loading. Figure 17. SEM of composite with 40% fibre loading.
 Fabrication and characterization of S. cilliare polymer composites 57

Table 4. Thermogravimetric analysis of RF, SC and P-Rnf-UF composites.

Sr. No. Sample code IDT (°C) % wt. loss FDT (°C) % wt. loss Final residue (%)

1. SC 212 12⋅45 471 67⋅44 32⋅66

2. R-F resin 299 22⋅64 990 51⋅78 48⋅22
3. P-Rnf-RF 248 14⋅49 943 57⋅37 57⋅48

Table 5. Differential thermal analysis of SC, RF and P-Rnf- Acknowledgements

UF composites.
Exothermic/endothermic peaks, We express our sincere thanks to Director, National Insti-
Sr. No. Sample code °C (μV) tute of Technology, Hamirpur, for providing basic labora-
tory facilities. Financial assistance from the University
1. SC 326⋅0 (81); 430⋅0 (203)
2. R-F resin 65 [–1⋅0]; 244 [8⋅0]; 280 [6⋅0] Grants Commission, New Delhi, through grant no.
3. P-Rnf-RF 81[–10⋅3] F.NO.-30-80/2004 (SR) is highly acknowledged.

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