Impact and Thermal Properties of Unsaturated Polyester (UPR) Composites Filled With Empty Fruit Bunch Palm Oil (EFBPO) and Cellulose
Advanced Materials Research: Editorial Board
AMR Editor(s) in Chief
Prof. Xiao Zhi Hu
University of Western Australia, School of Mechanical and Chemical Engineering
Perth, Australia, WA 6009
Prof. Alan Kin Tak Lau
Swinburne University of Technology, Faculty of Science, Engineering and Technology
John Street, Hawthorn, Australia, VIC 3122
AMR Editorial Board
Dr. Peng Cao
University of Auckland, Department of Chemical and Materials Engineering
Private Bag, Auckland, New Zealand, 92019
Prof. Ionel Chicinaş
Technical University of Cluj-Napoca, Faculty of Materials and Environmental Engineering,
Department of Materials Science and Engineering
103-105 Muncii Blv., Cluj-Napoca, 400641, Romania
Prof. Prafulla K. Jha
Maharaja Sayajirao University of Baroda, Department of Physics, Faculty of Science
Vadodara, India, 390 002
Prof. Heinz Palkowski
Clausthal University of Technology, Institute of Metallurgy
Robert-Koch-Strasse 42, Clausthal-Zellerfeld, 38678, Germany
Prof. Wolfgang Sand
University of Duisburg-Essen, Biofilm Centre, Aquatic Biotechnology
Geibelstrasse 41, Duisburg, 47057, Germany
Dr. Ching Hua Su
NASA/Marshall Space Flight Center, EM31 NASA/Marshall Space Flight Center
Huntsville, USA, 35812
Table of contents
Periodical:
Advanced Materials Research
Volume:
Advanced Materials Science and Technology
Papers published in this volume:
The Role and Prospect of Nanomaterials in Polymeric Membrane for Water and Wastewater
Treatment: A State-of-the-Art Overview
Ahmad Fauzi Ismail, Pei Sean Goh
p.3
Synthesis of Low Fouling Porous Polymeric Membranes
Heru Susanto, Dwi Putri Julyanti, Anis Roihatin
p.7
Mass Production of Stacked Styrofoam Nanofibers Using a Multinozzle and Drum Collector
Electrospinning System
Muhammad Miftahul Munir, Ade Yeti Nuryantini, Iskandar, Tri Suciati, Khairurrijal
p.20
Transparent and Conductive Fluorinated-Tin Oxide Prepared by Atmospheric Deposition
Technique
Agus Purwanto
p.24
Gas Sensing Using Static and Dynamic Modes Piezoresistive Microcantilever
Ratno Nuryadi, Lia Aprilia, Nuning Aisah, Djoko Hartanto
p.29
One-Step Fabrication of Short Nanofibers by Electrospinning: Effect of Needle Size on
Nanofiber Length
Indra Wahyudhin Fathona, Khairurrijal, Akihiro Yabuki
p.33
Carbon Dioxide Permeation Characteristics in Asymmetric Polysulfone Hollow Fiber
Membrane: Effect of Constant Heating and Progressive Heating
Muhamad Azwar Bin Azhari, Nooririnah Binti Omar, Nuzaimah Binti Mustaffa, Ahmad Fauzi Ismail
p.37
Electrospinning of Poly(vinyl alcohol)/Chitosan via Multi-Nozzle Spinneret and Drum
Collector
Ade Yeti Nuryantini, Muhammad Miftahul Munir, Muhamad Prama Ekaputra, Tri Suciati, Khairurrijal
p.41
A Simple Way of Producing Nano Anatase TiO2 in Polyvinyl Alcohol Fibers
Sabarman Harsojo, Kuwat Triyana, Harini Sosiati
p.45
Synthesis of Hydroxyapatite Nanoparticle from Tutut (Bellamya javanica) Shells by Using
Precipitation Method for Artificial Bone Engineering
Lenita Herawaty, Eti Rohaeti, Charlena, Sulistioso Giat Sukaryo
p.284
Adsorption of Lead Ions onto Citric Acid Modified Rubber (Hevea brasiliansis) Leaves
Shariff Ibrahim, Megat Ahmad Kamal Megat Hanafiah, Faisal Fadzil
p.288
Effect of Deacetylation on Characterization of pH Stimulus Responsive Chitosan-Acrylamide
Hydrogels Using Radiation
Kris Tri Basuki, Deni Swantomo, Sigit, Kartini Megasari
p.292
Synthesis of Smart Biodegradable Hydrogels Cellulose-Acrylamide Using Radiation as
Controlled Release Fertilizers
Deni Swantomo, Rochmadi, Kris Tri Basuki, Rahman Sudiyo
p.296
Structural Studies of 1,3:2,4-Dibenzylidene Sorbitol Gels
Hiroyuki Takeno, Yuta Kuribayashi
p.300
Effects of Surface Treatments on Nata de Cassava on the Tensile Strength and Morphology of
Bacterial Cellulose Sheet
Dini Cahyandari, Heru Santoso Budi Rohardjo
p.305
Impact and Thermal Properties of Unsaturated Polyester (UPR) Composites Filled with Empty
Fruit Bunch Palm Oil (EFBPO) and Cellulose
Elmer Surya, Michael, Halimatuddahliana, Maulida
p.310
Biodegradation of Low Density Polyethylene (LDPE) Composite Filled with Cellulose and
Cellulose Acetate
Halimatuddahliana, Ahmad Mulia Rambe
p.314
The Treated Rice Straw as Potentially Feedstock of Wood and Rice Straw Fiber Blend for Pulp
and Paper Making Industry
Ariadne L. Juwono, Handoko Subawi
p.318
Experimental Studies of Thermo-Induced Mechanical Effects in the Main-Chain Liquid Crystal
Elastomers
Supardi, Sabarman Harsojo, Yusril Yusuf
p.322
Advanced Materials Research Vol. 896 (2014) pp 310-313
© (2014) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/AMR.896.310
Impact and Thermal Properties of Unsaturated Polyester (UPR)
Composites Filled With Empty Fruit Bunch Palm Oil (EFBPO) and
Cellulose
Elmer Surya1, a, Michael1,b , Halimatuddahliana1,c , Maulida1,d
1
Department of Chemical Engineering, Universitas Sumatera Utara,
1-1-1-1 Jalan Almamater, Kampus USU Medan 20155, North Sumatra, Indonesia
a
elmer.surya@gmail.com, btrainsigma@hotmail.com
c
h_dahliana@yahoo.com, dmaulida70@gmail.com
Keywords: Unsaturated Polyester, EFBPO, Cellulose, Hand-Lay Up, Impact Test
Abstract. In this research, the impact properties of unsaturated polyester (UPR) composites filled
with empty fruit bunch palm oil (EFBPO) and cellulose are investigated. The composites were made
by hand-lay up method by mixing UPR with the content of each fillers (EFBPO and cellulose) of
5,10,15,20 wt.%. The parameter which was carried out on the prepared samples was impact test. It
was found that the addition of fillers to the matrix caused the impact strength of composites increased
at 10% addition of EFBPO and 5% addition of cellulose. The results are confirmed by fourier
transform infra-red (FTIR) and supported by thermogravimetric analysis (TGA) and scanning
electron microscopy (SEM).
Introduction
The study of polymer composites filled with natural fibers has increased rapidly. Natural
fibers provide a better property than synthetic fillers such as lower cost, high modulus and strength,
lower density, ease of fiber treatment and a wide range of application [1]. Also environmental
problem caused by and higher cost from synthetic fillers has led researchers to prefer natural fiber
over synthetic filler. The main component giving rise to these improve properties is cellulose. Several
natural fibers such as hemp, kenaf, kraft and jute has been investigated [1-4]. One commercial type of
matrix commonly used is unsaturated polyester (UPR). UPR is one of thermosets which possess
better properties than other types of thermoset such as low shrinkage, ability to mold at room
temperature, low viscosity, thermal and weather resistance, and low cost [5-8]. Other fillers
potentially of use are empty fruit bunch palm oil (EFBPO). As one of the largest country produced of
palm oil, Indonesia has plenty of EFBPO waste. If EFBPO could be treated further such as by
bleaching and pulping, then cellulose inside EFBPO could be extracted. The objective of this study is
to investigate the effect of filler contents on different types of fillers such as EFBPO and cellulose to
impact produced in the properties of composites.
Experimental Procedure
Materials Unsaturated Polyester Yukalac 157® BTQN-EX was supplied by PT. Justus Kimia
Raya Indonesia and empty fruit bunch palm oil (EFBPO) and cellulose was obtained from Indonesian
Oil Palm Research Institute. The matrix, unsaturated polyester (UPR) was mixed with the fillers with
content 5,10,15,20 wt% of each fillers (EFBPO and cellulose) by using hand lay-up method. The
catalyst used was methyl ethyl ketone peroxide (MEKP) acted as hardener for the matrix for 1,5 wt%
of the matrix. The curing period took 24 hours. The composites then were tested in accordance to
ASTM D4812-11 and carried out by GOTECH Impact Tester. The fracture of composite from impact
test then was analyzed by Scanning Electron Microscope (SEM) JEOL JSM-6360 LA. The data then
was supported by Fourier Transform Infra-Red (FTIR) using Shimadzu IR-Prestige 21 and
Thermogravimetric Analysis (TGA) using Shimadzu Simultaneous TGA/DTA Analyzer DTG-60.
All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP,
www.ttp.net. (ID: 114.79.37.53-08/02/14,17:18:27)
Advanced Materials Research Vol. 896
311
Results and Discussion
The impact properties of UPR-EFBPO and UPR-Cellulose composites is shown in Fig.1
Fig.1 shows that impact strength of
UPR-EFBPO composites increase as the fillers
content increase while the impact strength of
UPR-cellulose composites decreases. This is
happening due to absorption of UPR matrix by
cellulose during the mixing between both of
them to produce UPR-cellulose composites
while it was not found in mixing between UPR
and EFBPO. The cellulose fillers which
extracted from EFBPO have high pores
compared before EFBPO treatment of pulping
and bleaching hence its tendency to absorb
UPR would be higher than EFBPO. As the
cellulose content is increased to 20 wt%, the
Figure 1. Relationship Between Impact Strength
matrix cannot provide a sufficient area to hold
and Fillers Content
up the fillers, hence the interfacial adhesion
between matrix and fillers decreases which
results in the decreasing impact strength of UPR-cellulose composites as the fillers content increase.
The maximum impact strength is found at 5 % filler content. On the other hand, the impact strength of
UPR-EFBPO composites is found to increase as the fillers content increases where the maximum
value at 20% filler content. This shows that a good interfacial adhesion between matrix and fillers
occurs. The increased fillers make the composites more elastic and enhance the flexibility of network
in composites so it absorbs more
energy to failure [9-10].The
composites then were characterized
by Fourier Transform Infra-Red
(FTIR) as is shown by Fig.2.
Fig.2 shows the FTIR
characterization of the compounds
analyzed. It can be observed that the
IR spectrum of both composites
formed has a similar spectrum with
UPR matrix. Hence it shows that
mixing of matrix with the fillers does
not give any new peaks in the
composites. The interaction occurs
in the composites had been stated Figure 2. FTIR Analysis of: (a) UPR, (b) Cellulose, (c) EFBPO,
previously by Ray and Rout [8] such
(d) UPR-Cellulose, (e) UPR-EFBPO
as mechanical anchoring, interaction
between natural fillers and resin where –OH group in matrix (UPR) backbone provide an area to hold
hydrogen bonding with natural fillers which contain many hydroxyl groups inside and attractive
molecular forces (Van der Waals force and hydrogen bonding). The possibility interaction between
matrix and fillers is shown in Fig. 3. Since each of EFBPO and cellulose contains hydroxyl groups,
both of them would have similar interaction with the matrix.
Fig.4 shows the scanning electron microscope (SEM) analysis of impact fracture of composites. It
shows that the addition of fillers reduce the amount of void in the matrix. From both composites’
fracture, it shows the fiber pull out from the matrix. Fig.4 (b) and (c) shows the fiber pull out of
UPR-EFBPO composites and UPR-cellulose composites. In UPR-EFBPO composite, it can be seen
that the EFBPO fiber has more size diameter compared to cellulose in UPR-cellulose composite
which its fiber pull out consists of several fibrils. This form difference between EFBPO and cellulose
312
Advanced Materials Science and Technology
could lead in difference of energy absorbed in each of composites which EFBPO would absorb more
energy to break it down compare to cellulose. Therefore UPR-EFBPO composite must have higher
impact value than UPR-cellulose composites. The SEM analysis is shown in Fig.4.
Figure 3. Possibility Interaction Between Matrix and Natural Fillers [8]
Cellulose Fiber
Pull Out
Matrix
Matrix
Void
EFBPO Fiber
Pull Out
(a)
(b)
Matrix
(c)
Figure 4. Fracture Analysis of Scanning Electron Microscopy (SEM): (a) UPR (b) UPR-EFBPO (c)
UPR-Cellulose with Magnificent 500x
As addition data of this study, the thermo gravimetric analysis (TGA) of EFBPO, cellulose,
UPR-EFBPO 80/20 and UPR-cellulose 95/5 is done and shown in Fig.5.
Fig.5 shows that TGA curves of the materials exhibit three mass loss steps. The initial mass loss of
EFBPO and cellulose is below 225oC while for
UPR and both composites the initial mass loss
is below 325oC which is due to loss of volatile
material and loss of moisture [11]. In the
second step, the natural fibers are decomposed
due to degradation of its inside material to
become a volatile material [11] between 225oC
and 375oC. Meanwhile for UPR and both
composites, degradation of materials is due to
decomposition of matrix and fibers between
350oC-450oC. In the final step, natural fiber
has transformed into ash which marked by
constant mass loss while UPR and both
Figure 5. TGA Analysis of: (a) UPR, (b) EFBPO,
composites still have remain mass loss. The
(c) Cellulose, (d) UPR-EFBPO Composite, (e)
degradation is due to decomposition of
UPR-Cellulose Composite
aromatic chain, methane (CH4), CO2, and CO
release and structural rearrangements [12]. Table 1 gives the thermal data of TGA curves. From Table
1, it can be seen that UPR has more thermal stability compared to composites. This is due to
cross-linking process in UPR when cured process occurs, hence the polymer network becomes denser
and it needs more thermal energy to break down the network [9]. When natural fillers filled into the
matrix, it causes the thermal stability of composites formed decreases because the natural fillers have
low thermal stability. From both composites, it can be seen that UPR-cellulose composite has more
thermal stability than UPR-EFBPO composite due to its more degree of crystalline in cellulose than
EFBPO when EFBPO is having bleaching and pulping process produced cellulose.
Advanced Materials Research Vol. 896
313
Table 1. Thermal data of TGA curves of materials:
Materials
UPR
EFBPO
Cellulose
UPR-EFBPO 80/20
UPR-Cellulose 95/5
T10% [oC]
328,72
225
164,25
290,92
312,35
Tmax [oC]
450,13
348,63
391,62
426,1
445,03
Residue Weight at 500oC [%]
2,765
26,692
0,066
11,111
11,923
Conclusion
(1) UPR-EFBPO composites have higher impact strength than UPR-cellulose composites.
(2) In both composites formed, interaction occurs such as mechanical anchoring, hydrogen bonding
and Van der Waals forces.
(3) UPR still has the higher thermal stability than its composites due to “undisturbed” cross-linking in
polymer network
References
[1] H.N. Dhakal, Z.Y. Zhang, M.O.W. Richardson, Effect of water absorption on the mechanical
properties of hemp fibre reinforced unsaturated polyester composites, Composites Science and
Technology (2007,67), 1674-1683.
[2] M. R. Ishak, Z. Leman, S. M. Sapuan, A. M. M. Edeerozey and I. S. Othman, Mechanical
properties of kenaf bast and core fibre reinforced unsaturated polyester composites, IOP Conf.Series:
Materials Science and Engineering 11 (2010) 012006
[3] Zhenhua Gao, Dieying Ma, Xinying Lv, and Qingwen Wang, Formation and Evaluation of Kraft
Fibre-Reinforced Unsaturated Polyester (UPE) Composites, BioResources (2011) 6(4): 5167-5179
[4] D. Djeghader, B. Redjel, H. Hadidane, Impact Toughness of Composite Materials Jute-Polyester
and Glass-Polyester, 1st International Conference on Sustainable Built Environment Infrastructures in
Developing Countries ENSET Oran (Algeria) - October 12-14, 2009
[5] A.V.N. Prasad, K.M. Rao, G. Nagasrinivasulu, Mechanical Properties of banana empty fruit
bunch fibre reinforced polyester composites, Indian J. Fibre & Textile Research, (2009,34) 162-167
[6] B. Deepa, L.A. Pothan, R. Mavelil-Sam, S. Thomas, Structure, Properties and Recyclability of
Natural Fibre Reinforced Polymer Composites, Recent Developments in Polymer Recycling, (2011),
101-120.
[7] S. Waigaonkar, B.J.C. Babu, A. Rajput, Curing Studies of Unsaturated Polyester Resin Used in
FRP Products, Indian J. Engineering & Material Sciences, (2011,18), 31-39.
[8] D. Ray, J. Rout, Thermoset Biocomposites in A.K. Mohanty, M. Misra, L.T. Drzal, Natural
Fibers, Biopolymers, And Biocomposites. CRC Press: U.S.A. 2005, 305-306 & 313-315.
[9] A.H.P.S. Khalil, M.M. Marliana, T. Alshammari, Material Properties of Epoxy-Reinforced
Biocomposites With Lignin From Empty Fruit Bunch As Curing Agent, BioResources (2011) 6(4),
5206-5223.
[10] M. Khalid, C.T. Ratnam, T.G. Chuah, S. Ali, Thomas S.Y. Choong, Comparative study of
polypropylene composites reinforced with oil palm empty fruit bunch fiber and oil palm derived
cellulose, Elsevier Materials & Design (2006, 29), 173-178.
[11] S. Siyamak, N.A. Ibrahim, S. Abdolmohammadi, M.Z. Rahman, Enhancement of Mechanical
and Thermal Properties of Oil Palm Empty Fruit Bunch Fiber Poly(butylene adipate-co-terephtalate)
Biocomposites by Matrix Esterification Using Succinic Anhydride, Molecules (2012, 17),
1969-1991.
[12] M. Jawaid and A.H.P.S. Khalil, Effect of Layering Pattern on The Dynamic Mechanical
Properties and Thermal Degradation of Oil Palm-Jute Fibers Reinforced Epoxy Hybrid Composite,
BioResources (2011), 6(3), 2309-2322.
AMR Editor(s) in Chief
Prof. Xiao Zhi Hu
University of Western Australia, School of Mechanical and Chemical Engineering
Perth, Australia, WA 6009
Prof. Alan Kin Tak Lau
Swinburne University of Technology, Faculty of Science, Engineering and Technology
John Street, Hawthorn, Australia, VIC 3122
AMR Editorial Board
Dr. Peng Cao
University of Auckland, Department of Chemical and Materials Engineering
Private Bag, Auckland, New Zealand, 92019
Prof. Ionel Chicinaş
Technical University of Cluj-Napoca, Faculty of Materials and Environmental Engineering,
Department of Materials Science and Engineering
103-105 Muncii Blv., Cluj-Napoca, 400641, Romania
Prof. Prafulla K. Jha
Maharaja Sayajirao University of Baroda, Department of Physics, Faculty of Science
Vadodara, India, 390 002
Prof. Heinz Palkowski
Clausthal University of Technology, Institute of Metallurgy
Robert-Koch-Strasse 42, Clausthal-Zellerfeld, 38678, Germany
Prof. Wolfgang Sand
University of Duisburg-Essen, Biofilm Centre, Aquatic Biotechnology
Geibelstrasse 41, Duisburg, 47057, Germany
Dr. Ching Hua Su
NASA/Marshall Space Flight Center, EM31 NASA/Marshall Space Flight Center
Huntsville, USA, 35812
Table of contents
Periodical:
Advanced Materials Research
Volume:
Advanced Materials Science and Technology
Papers published in this volume:
The Role and Prospect of Nanomaterials in Polymeric Membrane for Water and Wastewater
Treatment: A State-of-the-Art Overview
Ahmad Fauzi Ismail, Pei Sean Goh
p.3
Synthesis of Low Fouling Porous Polymeric Membranes
Heru Susanto, Dwi Putri Julyanti, Anis Roihatin
p.7
Mass Production of Stacked Styrofoam Nanofibers Using a Multinozzle and Drum Collector
Electrospinning System
Muhammad Miftahul Munir, Ade Yeti Nuryantini, Iskandar, Tri Suciati, Khairurrijal
p.20
Transparent and Conductive Fluorinated-Tin Oxide Prepared by Atmospheric Deposition
Technique
Agus Purwanto
p.24
Gas Sensing Using Static and Dynamic Modes Piezoresistive Microcantilever
Ratno Nuryadi, Lia Aprilia, Nuning Aisah, Djoko Hartanto
p.29
One-Step Fabrication of Short Nanofibers by Electrospinning: Effect of Needle Size on
Nanofiber Length
Indra Wahyudhin Fathona, Khairurrijal, Akihiro Yabuki
p.33
Carbon Dioxide Permeation Characteristics in Asymmetric Polysulfone Hollow Fiber
Membrane: Effect of Constant Heating and Progressive Heating
Muhamad Azwar Bin Azhari, Nooririnah Binti Omar, Nuzaimah Binti Mustaffa, Ahmad Fauzi Ismail
p.37
Electrospinning of Poly(vinyl alcohol)/Chitosan via Multi-Nozzle Spinneret and Drum
Collector
Ade Yeti Nuryantini, Muhammad Miftahul Munir, Muhamad Prama Ekaputra, Tri Suciati, Khairurrijal
p.41
A Simple Way of Producing Nano Anatase TiO2 in Polyvinyl Alcohol Fibers
Sabarman Harsojo, Kuwat Triyana, Harini Sosiati
p.45
Synthesis of Hydroxyapatite Nanoparticle from Tutut (Bellamya javanica) Shells by Using
Precipitation Method for Artificial Bone Engineering
Lenita Herawaty, Eti Rohaeti, Charlena, Sulistioso Giat Sukaryo
p.284
Adsorption of Lead Ions onto Citric Acid Modified Rubber (Hevea brasiliansis) Leaves
Shariff Ibrahim, Megat Ahmad Kamal Megat Hanafiah, Faisal Fadzil
p.288
Effect of Deacetylation on Characterization of pH Stimulus Responsive Chitosan-Acrylamide
Hydrogels Using Radiation
Kris Tri Basuki, Deni Swantomo, Sigit, Kartini Megasari
p.292
Synthesis of Smart Biodegradable Hydrogels Cellulose-Acrylamide Using Radiation as
Controlled Release Fertilizers
Deni Swantomo, Rochmadi, Kris Tri Basuki, Rahman Sudiyo
p.296
Structural Studies of 1,3:2,4-Dibenzylidene Sorbitol Gels
Hiroyuki Takeno, Yuta Kuribayashi
p.300
Effects of Surface Treatments on Nata de Cassava on the Tensile Strength and Morphology of
Bacterial Cellulose Sheet
Dini Cahyandari, Heru Santoso Budi Rohardjo
p.305
Impact and Thermal Properties of Unsaturated Polyester (UPR) Composites Filled with Empty
Fruit Bunch Palm Oil (EFBPO) and Cellulose
Elmer Surya, Michael, Halimatuddahliana, Maulida
p.310
Biodegradation of Low Density Polyethylene (LDPE) Composite Filled with Cellulose and
Cellulose Acetate
Halimatuddahliana, Ahmad Mulia Rambe
p.314
The Treated Rice Straw as Potentially Feedstock of Wood and Rice Straw Fiber Blend for Pulp
and Paper Making Industry
Ariadne L. Juwono, Handoko Subawi
p.318
Experimental Studies of Thermo-Induced Mechanical Effects in the Main-Chain Liquid Crystal
Elastomers
Supardi, Sabarman Harsojo, Yusril Yusuf
p.322
Advanced Materials Research Vol. 896 (2014) pp 310-313
© (2014) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/AMR.896.310
Impact and Thermal Properties of Unsaturated Polyester (UPR)
Composites Filled With Empty Fruit Bunch Palm Oil (EFBPO) and
Cellulose
Elmer Surya1, a, Michael1,b , Halimatuddahliana1,c , Maulida1,d
1
Department of Chemical Engineering, Universitas Sumatera Utara,
1-1-1-1 Jalan Almamater, Kampus USU Medan 20155, North Sumatra, Indonesia
a
elmer.surya@gmail.com, btrainsigma@hotmail.com
c
h_dahliana@yahoo.com, dmaulida70@gmail.com
Keywords: Unsaturated Polyester, EFBPO, Cellulose, Hand-Lay Up, Impact Test
Abstract. In this research, the impact properties of unsaturated polyester (UPR) composites filled
with empty fruit bunch palm oil (EFBPO) and cellulose are investigated. The composites were made
by hand-lay up method by mixing UPR with the content of each fillers (EFBPO and cellulose) of
5,10,15,20 wt.%. The parameter which was carried out on the prepared samples was impact test. It
was found that the addition of fillers to the matrix caused the impact strength of composites increased
at 10% addition of EFBPO and 5% addition of cellulose. The results are confirmed by fourier
transform infra-red (FTIR) and supported by thermogravimetric analysis (TGA) and scanning
electron microscopy (SEM).
Introduction
The study of polymer composites filled with natural fibers has increased rapidly. Natural
fibers provide a better property than synthetic fillers such as lower cost, high modulus and strength,
lower density, ease of fiber treatment and a wide range of application [1]. Also environmental
problem caused by and higher cost from synthetic fillers has led researchers to prefer natural fiber
over synthetic filler. The main component giving rise to these improve properties is cellulose. Several
natural fibers such as hemp, kenaf, kraft and jute has been investigated [1-4]. One commercial type of
matrix commonly used is unsaturated polyester (UPR). UPR is one of thermosets which possess
better properties than other types of thermoset such as low shrinkage, ability to mold at room
temperature, low viscosity, thermal and weather resistance, and low cost [5-8]. Other fillers
potentially of use are empty fruit bunch palm oil (EFBPO). As one of the largest country produced of
palm oil, Indonesia has plenty of EFBPO waste. If EFBPO could be treated further such as by
bleaching and pulping, then cellulose inside EFBPO could be extracted. The objective of this study is
to investigate the effect of filler contents on different types of fillers such as EFBPO and cellulose to
impact produced in the properties of composites.
Experimental Procedure
Materials Unsaturated Polyester Yukalac 157® BTQN-EX was supplied by PT. Justus Kimia
Raya Indonesia and empty fruit bunch palm oil (EFBPO) and cellulose was obtained from Indonesian
Oil Palm Research Institute. The matrix, unsaturated polyester (UPR) was mixed with the fillers with
content 5,10,15,20 wt% of each fillers (EFBPO and cellulose) by using hand lay-up method. The
catalyst used was methyl ethyl ketone peroxide (MEKP) acted as hardener for the matrix for 1,5 wt%
of the matrix. The curing period took 24 hours. The composites then were tested in accordance to
ASTM D4812-11 and carried out by GOTECH Impact Tester. The fracture of composite from impact
test then was analyzed by Scanning Electron Microscope (SEM) JEOL JSM-6360 LA. The data then
was supported by Fourier Transform Infra-Red (FTIR) using Shimadzu IR-Prestige 21 and
Thermogravimetric Analysis (TGA) using Shimadzu Simultaneous TGA/DTA Analyzer DTG-60.
All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP,
www.ttp.net. (ID: 114.79.37.53-08/02/14,17:18:27)
Advanced Materials Research Vol. 896
311
Results and Discussion
The impact properties of UPR-EFBPO and UPR-Cellulose composites is shown in Fig.1
Fig.1 shows that impact strength of
UPR-EFBPO composites increase as the fillers
content increase while the impact strength of
UPR-cellulose composites decreases. This is
happening due to absorption of UPR matrix by
cellulose during the mixing between both of
them to produce UPR-cellulose composites
while it was not found in mixing between UPR
and EFBPO. The cellulose fillers which
extracted from EFBPO have high pores
compared before EFBPO treatment of pulping
and bleaching hence its tendency to absorb
UPR would be higher than EFBPO. As the
cellulose content is increased to 20 wt%, the
Figure 1. Relationship Between Impact Strength
matrix cannot provide a sufficient area to hold
and Fillers Content
up the fillers, hence the interfacial adhesion
between matrix and fillers decreases which
results in the decreasing impact strength of UPR-cellulose composites as the fillers content increase.
The maximum impact strength is found at 5 % filler content. On the other hand, the impact strength of
UPR-EFBPO composites is found to increase as the fillers content increases where the maximum
value at 20% filler content. This shows that a good interfacial adhesion between matrix and fillers
occurs. The increased fillers make the composites more elastic and enhance the flexibility of network
in composites so it absorbs more
energy to failure [9-10].The
composites then were characterized
by Fourier Transform Infra-Red
(FTIR) as is shown by Fig.2.
Fig.2 shows the FTIR
characterization of the compounds
analyzed. It can be observed that the
IR spectrum of both composites
formed has a similar spectrum with
UPR matrix. Hence it shows that
mixing of matrix with the fillers does
not give any new peaks in the
composites. The interaction occurs
in the composites had been stated Figure 2. FTIR Analysis of: (a) UPR, (b) Cellulose, (c) EFBPO,
previously by Ray and Rout [8] such
(d) UPR-Cellulose, (e) UPR-EFBPO
as mechanical anchoring, interaction
between natural fillers and resin where –OH group in matrix (UPR) backbone provide an area to hold
hydrogen bonding with natural fillers which contain many hydroxyl groups inside and attractive
molecular forces (Van der Waals force and hydrogen bonding). The possibility interaction between
matrix and fillers is shown in Fig. 3. Since each of EFBPO and cellulose contains hydroxyl groups,
both of them would have similar interaction with the matrix.
Fig.4 shows the scanning electron microscope (SEM) analysis of impact fracture of composites. It
shows that the addition of fillers reduce the amount of void in the matrix. From both composites’
fracture, it shows the fiber pull out from the matrix. Fig.4 (b) and (c) shows the fiber pull out of
UPR-EFBPO composites and UPR-cellulose composites. In UPR-EFBPO composite, it can be seen
that the EFBPO fiber has more size diameter compared to cellulose in UPR-cellulose composite
which its fiber pull out consists of several fibrils. This form difference between EFBPO and cellulose
312
Advanced Materials Science and Technology
could lead in difference of energy absorbed in each of composites which EFBPO would absorb more
energy to break it down compare to cellulose. Therefore UPR-EFBPO composite must have higher
impact value than UPR-cellulose composites. The SEM analysis is shown in Fig.4.
Figure 3. Possibility Interaction Between Matrix and Natural Fillers [8]
Cellulose Fiber
Pull Out
Matrix
Matrix
Void
EFBPO Fiber
Pull Out
(a)
(b)
Matrix
(c)
Figure 4. Fracture Analysis of Scanning Electron Microscopy (SEM): (a) UPR (b) UPR-EFBPO (c)
UPR-Cellulose with Magnificent 500x
As addition data of this study, the thermo gravimetric analysis (TGA) of EFBPO, cellulose,
UPR-EFBPO 80/20 and UPR-cellulose 95/5 is done and shown in Fig.5.
Fig.5 shows that TGA curves of the materials exhibit three mass loss steps. The initial mass loss of
EFBPO and cellulose is below 225oC while for
UPR and both composites the initial mass loss
is below 325oC which is due to loss of volatile
material and loss of moisture [11]. In the
second step, the natural fibers are decomposed
due to degradation of its inside material to
become a volatile material [11] between 225oC
and 375oC. Meanwhile for UPR and both
composites, degradation of materials is due to
decomposition of matrix and fibers between
350oC-450oC. In the final step, natural fiber
has transformed into ash which marked by
constant mass loss while UPR and both
Figure 5. TGA Analysis of: (a) UPR, (b) EFBPO,
composites still have remain mass loss. The
(c) Cellulose, (d) UPR-EFBPO Composite, (e)
degradation is due to decomposition of
UPR-Cellulose Composite
aromatic chain, methane (CH4), CO2, and CO
release and structural rearrangements [12]. Table 1 gives the thermal data of TGA curves. From Table
1, it can be seen that UPR has more thermal stability compared to composites. This is due to
cross-linking process in UPR when cured process occurs, hence the polymer network becomes denser
and it needs more thermal energy to break down the network [9]. When natural fillers filled into the
matrix, it causes the thermal stability of composites formed decreases because the natural fillers have
low thermal stability. From both composites, it can be seen that UPR-cellulose composite has more
thermal stability than UPR-EFBPO composite due to its more degree of crystalline in cellulose than
EFBPO when EFBPO is having bleaching and pulping process produced cellulose.
Advanced Materials Research Vol. 896
313
Table 1. Thermal data of TGA curves of materials:
Materials
UPR
EFBPO
Cellulose
UPR-EFBPO 80/20
UPR-Cellulose 95/5
T10% [oC]
328,72
225
164,25
290,92
312,35
Tmax [oC]
450,13
348,63
391,62
426,1
445,03
Residue Weight at 500oC [%]
2,765
26,692
0,066
11,111
11,923
Conclusion
(1) UPR-EFBPO composites have higher impact strength than UPR-cellulose composites.
(2) In both composites formed, interaction occurs such as mechanical anchoring, hydrogen bonding
and Van der Waals forces.
(3) UPR still has the higher thermal stability than its composites due to “undisturbed” cross-linking in
polymer network
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