Mechanical, thermal and water absorption properties of

woven okra fiber polyester composites

D.K. NAGESWARA RAO1*, K. RAJA NARENDER REDDY2, T.RAMU3,
K. GOPALA KISHAN RAO4 AND KAMAL K. KAR5
1
BVC Institute of Technology & Science, Amalapuram- 533 201, India
2
Department of Mechanical Engineering, Kakatiya Inst of Technology & Science Warangal-506 015 India
3
Department of Mechanical Engineering, SRR Engineering College, Khammam-507 123, India
4
Central Instrumentation Centre, Kakatiya University, Warangal-506 009, India
5
Advanced Nanoengineering Materials Laboratory, Indian Institute of Technology, Kanpur-208016, India
*
Corresponding author: [email protected] Cell: 91-9393399960, Fax: 91-8856-235489

ABSTRACT: Okra fiber reinforced polyester composites are made of woven

unidirectional mats with treated and untreated fibers. The composites are tested for
tensile, flexure and impact properties and water absorption behavior. Higher flexure
modulus and impact strengths are obtained for untreated okra fiber composite while
superior flexure and tensile strengths, high tensile modulus and low water absorption
characteristics are obtained for the treated fiber composite. The DSC analysis has given
high glass transition temperature for the untreated fiber composite. Morphological studies
through SEM revealed a brittle fracture for the treated fiber composite and traces of fiber
pull out are observed for the untreated fiber composite.

KEY WORDS: Natural fiber composites, Mechanical properties, Surface treatments,

DSC analysis, SEM analysis.

INTRODUCTION

The okra plant [1] shown in Fig. 1a. is of African or Asian origin and it belongs to the
Malvaceae family. This is an annual herb having a 3-7 ft. high stem, covered with hairs
and leaves and it is grown as a garden crop or home yard plant throughout the tropical
and subtropical parts of the world. This plant is generally having edible, medicinal and
other uses. Tender pods are used as vegetable. Root is edible but is very fibrous and
mucilaginous, having a strongly demulcent action.
Okra plant is popular for its long and soft fibers. Kenaf also belongs to the same
family and studies on kenaf fiber composites are available in the literature but no
significant work has been reported on okra fiber composites. Wambua, et al [2] have
investigated the mechanical properties of sisal, kenaf, hemp, jute and coir reinforced
polypropylene composites. Feng, et al [3] have studied the structure-property
relationships of kenaf fiber reinforced polypropylene composites. To increase the
adhesion between the hydrophilic fibers and hydrophobic matrix, Maya [4,5] has
suggested the alkali treatment as one of the most common and efficient methods of
chemical modification.
The influence of chemical treatment on flexure, tensile and impact strengths, as
well as thermal and water absorption properties are evaluated for woven okra fiber
composites. The results are also compared with those available for kenaf fiber
composites. SEM study is made to visualize the nature of fracture and the influence of
chemical treatment on fracture behavior.

MATERIALS AND TESTING

Fibers
To extract a useful fiber, the stalks are collected green after fruiting and are
subjected to water retting process. The fibers are about 2.4m long and are shown in Fig.
1b. These fibers are also used in making paper and textiles.

Fiber modifications
For chemical treatment, the dried fibers are soaked in 2% NaOH solution for 24
hrs at room temperature. This treatment helps in dissolving lignin and hemicelluloses and
to expose more of the fiber OH groups. The fibers are washed thoroughly with double
distilled water to remove NaOH. These treated fibers are dried at room temperature for
24 hours and are shown in Fig. 1c.

Preparation of composites
 Unidirectional mats shown in Fig. 2 are prepared on an indigenous weaving set up
using the treated and untreated fibers. General purpose isopthalic polyester resin procured
from M/s Sakthi Fiber Glass, Chennai, India, is used for preparing the composites. 2%
MEKP and 2% cobalt napthalate are used as additives. Wax polish and ploy vinyl alcohol
(PVA) are used as releasing agents. The composites are fabricated in an open mold
process between two thick glass plates. To create a thin separating layer, wax polish is
applied on the glass plates with a subsequent coat of PVA. The lamina is prepared with a
matrix fiber ratio of 6.

Flexure, tensile and impact tests

To obtain the flexure properties, the three-point bend test is conducted as per
ASTM D-790 using a compression testing machine supplied by Hydraulic and
Engineering Instruments, New Delhi, with cross head speed of 1.25 mm/minute. The
tensile test is conducted as per ASTM D-698 on Zwick / Roell Z010 10KN at a cross
head speed of 3mm/min. The standard Type IV dumb bell shaped specimens are used in
the testing. Notched impact performance of the composite is evaluated as per ASTM D-
256 using Izod impact supplied by PSI Sales Pvt.Ltd., New Delhi. This test method
elaborates the determination of the resistance to breakage by flexural shock. Five
specimens are used for each type of test.

Morphology
Morphology of the fractured surfaces and the fiber pull out are studied by
Scanning Electron Microscopy (SEM) using EVOMA15 Smart SEM.

Water absorption test

The water absorption test is conducted as per ASTM D-579 on rectangular
specimens of 25.4  76.2 mm2 size with untreated and treated fibers. The samples are
conditioned by heating in an oven at 50 oC for 24 hours and cooling. The weights of the
samples are taken by Shimadzu Electronic Balance with readability of 0.001g. All the
samples are immersed in double distilled water for 24 hrs at room temperature. The
percentage increase in weight of the specimens during immersion is obtained by taking
the ratio of increase in average weight of the conditioned specimen after immersion in
water for 24 hrs and the average weight of conditioned specimen calculated nearest to
0.01%. All the samples are reconditioned by keeping them in oven for 24 hrs at 50 oC.
The amount of soluble matter lost is given by the decrease in weight of the specimen after
reconditioning.

Differential scanning calorimetry (DSC)

Composites exhibit changes in material properties such as volume, enthalpy, heat
capacity, thermal expansion and tensile modulus as the material is heated through the
glass transition temperature, Tg and goes from glass to rubbery state. The DSC is
performed with the help of Mettler using Star SW 8.1 analyzer to measure Tg.

RESULTS AND DISCUSSION

Flexure strength
The load-deflection diagram for flexure test on okra fiber composites is shown in
Fig. 3. Table 1 gives the values of flexure strength, flexure modulus and tensile strength
and tensile modulus of untreated and treated okra fiber composites and the results of
kenaf fiber composites available in the literature. For untreated okra fiber composite, the
flexure strength is 156.93 MPa with fibers, and it is equal to 208.84 MPa for the treated
fiber composite. The flexure strength for neat resin is 136.35 MPa. The flexure strength
of kenaf/polypropylene composite with 30% fiber-volume fraction [2] is 30 MPa. The
flexure strength of treated okra fiber composite is 1.53 times that of neat resin and 1.33
times that of untreated fiber composite. The untreated okra fiber composite has the
highest flexure modulus equal to 32726 MPa which is 4.55 times that of neat resin. The
treated fiber composite has lower flexure modulus equal to 30070 MPa which is 0.92
times that of the untreated fiber composite. The flexure modulus for kenaf/polypropylene
composite [2] is equal to 2100 MPa which is much less than that of neat resin.
Reinforcement by untreated okra fibers has slightly increased the flexure strength
compared to neat resin. However, the increase is significant in case of treated fiber
composite. The untreated okra fiber composite has the highest flexure modulus. It
indicates that chemical treatment has not increased the flexure modulus although it has
increased the flexure strength. Increased adhesion between the fibers and the matrix has
increased the stiffness of the composite causing brittle fracture during bending and
resulted in lower flexure modulus. The specific flexural strength and specific flexural
modulus of the composites and the neat resin are shown in Figs. 4 and 5. The fractured
surface of untreated okra fiber composite is shown in Fig. 6 and fiber pull out due to
weak adhesion is visible. Brittle fracture is observed in SEM micrograph shown in Fig. 7.

Morphology
The SEM micrographs of the fractured surfaces of untreated and treated
unidirectional okra fiber composites are shown in Figs. 6 and 7 respectively. The fracture
surface of untreated fiber composite in Fig. 6 shows fiber pullout in certain region
indicating a weak interface bonding while sharp fracture of all the fibers and a strong
interfacial bonding between the fiber and matrix can be observed in Fig. 7.

Tensile strength

The load-deflection diagrams and the stress-strain curves are shown in Figs. 8 and
9 respectively. The values of ultimate tensile strength and the tensile modulus of
untreated and treated okra fiber composites are shown in Table 1. Highest ultimate
tensile strength of 113.6 MPa is obtained for treated fiber composite while for untreated
fiber composite, it is equal to 69.78 MPa and for neat resin, it is 38.5 MPa. The treated
fiber composite has 2.95 times higher tensile strength than that of neat resin and 1.63
times that of untreated fiber composite. The tensile strength of kenaf/polypropylene
composite is 30 MPa with 30% fiber-volume fraction [2] and it is equal to 33.3 MPa for
kenaf/polypropylene composite with 50% fiber-volume fraction [3]. Treated okra fiber
composite has exhibited the highest tensile modulus of 2785 MPa. It is 6.98 times that of
neat resin and 1.2 times that of untreated fiber composite. Higher tensile modulus equal
to 6800 MPa is obtained for kenaf/polypropylene composite with 30% fiber-volume
fraction [2], and a much higher value is equal to 9300 MPa is obtained for
kenaf/polypropylene composite with 50% fiber-volume fraction [3]. The
kenaf/polypropylene composites have extremely superior tensile modulus property
compared to that of okra/polyester composites. The specific tensile strength and specific
tensile moduli for different okra fiber composites are shown in Figs. 10 and 11
respectively.

Impact strength
The untreated okra fiber composite has exhibited highest impact strength. For the
untreated fiber composite, it is equal to 22.97 kJ/m 2 and for the treated fiber composite, it
is 20.25 kJ/m2. Higher impact strength of the untreated okra fiber composite can be
attributed to its higher flexure modulus. The impact strength of neat resin is 1.89 kJ/m 2.
These values are shown in Fig.12. For kenaf/polypropylene composites [2], the impact
strength is 14 kJ/m2. This is less compared to those of treated and untreated okra fiber
composites.

Water absorption

Treatment of okra fibers with NaOH for 24 hrs has made the fibers less
hydrophilic and decreased the water absorption capacity by 61%. The treated okra fiber
composite has absorbed less water compared to the untreated composite and the moisture
absorption behavior is shown in Fig. 13. As the fibers are hydrophilic in nature, they
absorb water during immersion and upon reconditioning, loss of matter is observed. The
percentage loss of soluble matter during immersion after reconditioning the specimens is
shown in Fig.14. The loss is present for the untreated composite. But, for the treated
composite less loss is observed. This can be attributed to the formation of protective layer
in the fiber-matrix interface that prevented the loss of soluble matter. Absorption of water
by lignocellulose material has formed hydrogen bonds between water and hydroxyl
groups of cellulose, hemicellulose and lignin in the cell wall [4] and caused swelling.
This has resulted in increase in thickness and reduction in length. Increase in thickness is
due to less constraint on outer surface compared to the constraint offered by matrix and
adjacent fibers in the direction of the width. Less water absorption by treated composites
is due to replacement of hydrophilic OH groups of fiber by more hydrophobic ester
groups or due to formation of a protective layer on the interfacial zone which prevented
water molecules from penetrating in to the cell wall. The moisture absorption behavior
for long-time immersion up to 1200 hours is shown in Fig. 15. It can be noted that there
is a gradual increase in water absorption up to 950 hours and it has decreased later. The
change in weight, thickness, width and length due to long time immersion are shown in
Figs. 16-18.

DSC Analysis
The thermal behavior of century fiber reinforced composite in nitrogen
atmosphere of 30ml/min with a heating rate of 10oC during temperature range of 25-
150oC for okra fiber composites as well as for neat resin are shown in Fig.19-20. For
composite with untreated fibers, the first peak is observed at 74.41 oC as in Fig. 19. For
composite with treated fibers, the peak is at 73.91 oC as in Fig. 20. For neat resin, the
peak is observed at 73.4oC as shown in Fig. 21. These peaks indicate the glass transition
temperature Tg. Increase in Tg represents reduction of mobility of the polymer backbone
due to formation of chemical bond between the resin and the matrix. Higher T g of treated
fiber composite indicates higher thermal stability compared to untreated fiber composite
and the neat resin.

CONCLUSION
Untreated okra fiber composite has higher flexure modulus and impact strength
and better glass transition temperature. The treated fiber composite has superior flexure
and tensile strengths and tensile modulus properties and reduced water absorption
characteristic. SEM studies revealed a brittle fracture for the treated fiber composite and
traces of fiber pull out are noticed for the untreated fiber composite due to weak fiber
matrix bonding.

ACKNOWLEDGEMENTS
Financial support by A.P. State Council for Science and Technology (APCOST),
Warangal Regional Centre, Hyderabad, India, vide letter APCOST/wgl/s&t/SPP/2007-
2008 dated 31.3.2008 is gratefully acknowledged.
REFERENCES
1. The Wealth of India-A Dictionary of Indian raw materials and industrial products,
Raw materials, vol. V, CSIR, New Delhi, 1959, pp. 84-88.
2. Wambua, P., Ivens, J. and Verpoest, I. (2003), Natural fibers: can they replace glass
fibre reinforced plastics?, Composites Science and Technology, 63: 1259-1264.

3. Feng, D., Caulfield, D.F. and Sanadi, A.R. (2001), Effect of compatibilizer on the
structure-property relationships of kenaf-fiber/polypropylene composites, Polym
Compos. 22(4): 506-517.
4. Maya, J.J. and Rajesh, D.A. (2008). Recent developments in chemical modifications
and characterization of natural fiber composites, Polym Compos. 29: 187-207.
5. Maya, J.J., Bejoy, F., Varughese, K.T. and Thomas, S. (2008). Effect of chemical
modification on properties of hybrid biocomposites, Composites: Part A, 39: 352-
362.

FIGURE CAPTIONS
Figure 1. (a) Okra plant (b) untreated fiber (c) treated fiber
Figure 2. Woven okra fiber mats (a)untreated fiber (b)treated fiber
Figure 3. Flexure load-deflection diagram
Figure 4. Specific flexure strength of okra composites
Figure 5. Specific flexure modulus of okra composites
Figure 6. SEM image of untreated unidirectional composite
Figure 7. SEM image of treated unidirectional composite
Figure 8. Tensile load-deflection diagram of okra composites
Figure 9. Tensile stress-strain diagram of okra composites
Figure 10. Specific tensile strength of okra composites
Figure 11. Specific tensile modulus of okra composites
Figure 12. Impact strength of okra fiber composites
Figure 13. Moisture absorption behavior of okra composites
Figure 14. Soluble matter lost
Figure 15. Moisture absorption behavior due to long-time immersion
Figure 16. Change in thickness due to long-time immersion
Figure 17. Change in width due to long-time immersion
Figure 18. Change in length due to long-time immersion
Figure 19. Thermogram for untreated woven okra fiber composite (UT-UD)
Figure 20. Thermogram for treated woven okra fiber composite (T-UD)
Figure 21. Thermogram for isopthalic resin

CAPTIONS FOR TABLES

Table 1. Comparison of flexure, tensile and impact properties of okra and kenaf fiber
composites

Property(MPa) utofc tofc neat resin Wambua[2] Feng [3]

Flexure strength 156.93 208.84 136.35 30 -
Flexure modulus 32726 30070 7191 2100 -
Ultimate tensile
strength 69.78 113.6 38.5 30 33.3
Tensile modulus 2311 2785 398.6 6800 9300
Impact strength -
( kJ/m2) 22.97 20.25 1.89 14*
Density (g/cm3) 1.196133 1.285138 1.265101 - -
Table 1.
utofc-untreated okra fiber composite tofc-treated okra fiber composite
[2]-kenaf/polypropylene-30% fiber volume fraction [3]- kenaf/polypropylene 50% fiber volume fraction, *Charpy impact