UNIVERSITI PUTRA MALAYSIA
CHARACTERIZATION OF NANOCOMPOSITES BASED ON PLASTICIZED STARCH AND KENAF BAST NANOFIBERS
SAMANEH KARIMIMAZRAEHSHAHI
IPTPH 2014 1
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CHARACTERIZATION OF NANOCOMPOSITES BASED ON
PLASTICIZED STARCH AND KENAF BAST NANOFIBERS
By
SAMANEH KARIMIMAZRAEHSHAHI
Thesis Submitted to the School of Graduate Studies, Universiti Putra
Malaysia, in Fulfillment of the Requirements for the Degree of Doctor of
Philosophy
January 2014
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COPYRIGHT
All material contained within the thesis, including without limitation text, logos,
icons, photographs and all other artwork, is copyright material of Universiti Putra
Malaysia unless otherwise stated. Use may be made of any material contained
within the thesis for non-commercial purposes from the copyright holder.
Commercial use of material may only be made with the express, prior, written
permission of Universiti Putra Malaysia.
Copyright © Universiti Putra Malaysia
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DEDICATION
I dedicate this dissertation to my wonderful family who surrounds me with
unconditional LOVE.
Especially to:
My lovely husband, Mehdi, who is always pushing me forward and is the source
of energy, inspiration and courage.
My uncle, Professor Ali, who without his encouragements, sacrifices and support
this work was not possible.
My terrific parents, Ashraf & Hassan, who are the source of love and compassion.
I never would have made it here without you!
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Abstract of thesis presented to the Senate of Universiti Putra Malaysia in
fulfilment of the requirement for the degree of Doctor of Philosophy
CHARACTERIZATION OF NANOCOMPOSITES BASED ON
PLASTICIZED STARCH AND KENAF BAST NANOFIBERS
By
SAMANEH KARIMIMAZRAEHSHAHI
January 2014
Chair: Professor Paridah Md. Tahir, PhD
Institute: Institute of Tropical Forestry and Forest Products
Plants cell walls are biological nanocomposites which exhibit high mechanical
properties at a light weight. The secret of this rigidity and strength lies in its main
structural component; cellulose. Native cellulose exists as highly-ordered
microfibrils, which are just a few nanometers wide and have been found to be
stiffer than many synthetic fibers. Many critical issues associated with global
warming, environmental pollution and the amount of plastic wastes, synergistic
with the scarcity and non-renewability of petroleum and petroleum-based products
are driving material and composite scientists to focus on development of
renewable and sustainable biomaterials. In this quest, using cellulose microfibrils
from plant materials as renewable alternatives to conventional reinforcement
materials such as glass fibers and carbon fibers is generating particular interest.
Cellulosic nanofibers have the potential to reinforce and enhance properties of
polymeric matrices, significantly, even at very low volume fractions. According to
objectives of this research, by applying a chemi-mechanical approach both
unbleached and bleached cellulose nanofibers were extracted from the cell wall of
kenaf bast fibers and characterized. Then, the reinforcement performances of
these two nanofillers were studied and compared using the starch as a matrix
material, to identify the necessity of bleaching procedures in nanofiber isolation
process. Subsequently, according to result, nanocomposite with different fiber
loadings were prepared with unbleached nanofibers. Structural and mechanical
performances of these materials were studied and compared with the composite
prepared with micro scale cellulosic fibers from kenaf bast, unders the same
conditions, to fully understand the effect of fibers loading and dimension on
properties of fabricated materials.
In order to undertake the research objectives, cellulosic fiber hierarchy from kenaf
bast were isolated in three stages. Initially raw kenaf bast fibers were subjected to
soda-AQ pulping process to eliminate lignin and hemicellulose. Unbleached fibers
then undergone a bleaching process and finally both pulped and bleached fibers
were mechanically separated into their constituent nanoscale cellulosic fibers. The
influence of each treatment on the chemical composition, morphology, functional
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groups, crystallinity, and thermal stability of fibers was investigated. Attenuated
total reflectance Fourier transform infrared spectroscopy (ATR/FTIR) showed that
lignin and hemicellulose were almost entirely removed during the alkali and
bleaching treatments. Morphological studies of fiber hierarchy were done by
scanning electron microscopy (SEM) and transmission electron microscopy
(TEM). X-Ray diffraction (XRD) analysis revealed that the crystallinity of fibers
increased from 62.9 to 81.5% as subsequent treatments were applied. Comparison
with other works demonstrated the effectiveness and superior yield of 62.5% for
unbleached nanofibers and 58% for bleached nanofibers, in the applied approach
for producing nanocellulose from kenaf bast fibers. The isolated nanofibers
displayed about 10% enhancement in thermal stability compare to that of raw
kenaf bast fiber. The results of study on the properties of isolated bleached and
unbleached nanofibers indicated the probable redundancy of the bleaching process
as no significant difference was observed in their characteristics.
The surface chemistry of the unbleached and bleached nanofibers is different and
it has led to different behavior when these nanofibers are incorporated into
polymeric matrices. In order to evaluate this issue both types of nanofibers were
used to reinforce thermoplastic starch matrix and properties of obtained
nanocomposite films were characterized using SEM, ATR/FTIR, XRD,
thermogravimetric analysis (TGA), tensile and water uptake experiments. The
results showed superior overall performance of nanocomposite films made from
unbleached nanofibers. Thus the redundancy of bleaching procedures in nanofiber
isolation process was cleared.
In the subsequent work, unbleached nanofibers with different loading (0-10 wt%)
were incorporated into thermoplastic starch matrix. Thin bionanocomposite films
were made by casting and evaporating the mixture of aqueous suspension of
nanofibers, starch and glycerol which underwent gelatinization process at the
same time. In order to elucidate the importance and the effect of nanoscale
cellulosic fibers on the performance of fabricated materials, starch based
composite films with the exact same conditions were made by using micro sized
pulverized kenaf bast fibers. The resulting composite and nanocomposite films
were characterized by SEM, TEM, ATR/FTIR, XRD, TGA, scanning differential
calorimetry (DSC), dynamic mechanical thermal analysis (DMTA), tensile and
water uptake experiments. Among tested materials, the nanoreinforced composites
had significantly greater performance, particularly; increased mechanical strength
and reduced water sensitivity. Tensile strength and Young’s modulus increased by
313% and 343% and water uptake reduced by 21% with addition of 10%
nanofibers. Overalls results demonstrated that applied nanofibers strongly
interacted by hydrogen bonding with the starch matrix and showed a favourable
compatibility which can be attributed to their chemical similarities.
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Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia
Sebagai memenuhi keperluan untuk ijazah Doktor Falsafah
PENCIRIAN NANOKOMPOSIT BERDASARKAN DIPLASTIKKAN
KANJI DAN KENAF BAST NANOFIBERS
Oleh
SAMANEH KARIMIMAZRAEHSHAHI
Januari 2014
Pengerusi: Professor Paridah Md. Tahir, PhD
Institut: Institut Perhutanan Tropika dan Produk Hutan
Dinding sel tumbuhan nanokomposit biologi yang menunjukkan sifat-sifat
mekanik yang tinggi pada berat cahaya. Rahsia ketegaran dan kekuatan terletak
kepada komponen utamanya iaitu struktur selulosa.Selulosa asli microfibrils yang
wujud sangat tinggi, yang mempunyai luas hanya beberapa nanometer telah
didapati lebih keras daripada banyak serat sintetik. Banyak isu-isu kritikal yang
berkaitan dengan pemanasan global, pencemaran alam sekitar dan jumlah sisa
plastik, yang disinergi dengan kekurangan dan petroleum yang tidak diperbaharui
dan produk berasaskan petroleum dalam pembangunan bahan komposit dan
saintis memberi tumpuan kepada pembangunan biobahan yang boleh diperbaharui
dan mudah diperolehi. Dalam usaha ini, dengan menggunakan microfibrils
selulosa dari bahan tumbuhan sebagai alternatif yang boleh diperbaharui kepada
bahan-bahan pengukuhan konvensional seperti gentian kaca dan gentian karbon
adalah menjana kepentingan tertentu. Nanofibers Cellulosic mempunyai potensi
untuk mengukuh dan meningkatkan sifat-sifat matriks polimer, dengan ketara,
walaupun pada pecahan jumlah yang sangat rendah. Menurut objektif kajian ini,
dengan menggunakan pendekatan bahan- mekanikal kedua-dua luntur dan
terluntur nanofibers selulosa dipetik daripada dinding sel kenaf fibers. Kemudian,
prestasi pengukuhan kedua-dua nanofillers telah dikaji dan dibandingkan
menggunakan kanji sebagai bahan matriks, untuk mengenal pasti keperluan
prosedur pelunturan dalam proses pengasingan nanofiber. Selepas itu, menurut
hasil, nanocomposite dengan bebanan gentian yang berbeza telah disediakan
dengan nanofiber luntur. Prestasi struktur dan mekanikal bahan-bahan ini telah
dikaji dan dibandingkan dengan komposit yang disediakan dengan skala mikro
serat cellulosic dari kenafbast, dalam keadaan yang sama, untuk memahami
sepenuhnya kesan serat memuatkan dan dimensi pada sifat bahan fabrikasi.
Dalam kajian ini, hirarki gentian selulosa dari kulit kenaf telah diasingkan dalam
tiga peringkat yang berbeza. Gentian kulit kenaf mentah pada mulanya telah
melalui proses pempulpaan untuk mengasingkan lignin dan hemiselulosa. Setelah
mendapatkan gentian daripada pulpa, ia melalui proses pelunturan dan akhirnya
kedua-dua gentian pulpa dan gentian yang telah dilunturkan diasingkan secara
mekanikal kepada konstituen gentian selulosa berskalanano. Kesan setiap rawatan
terhadap kandungan kimia, morfologi, kumpulan fungsi, kristaliniti, dan
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kestabilan haba gentian telah dikaji. Jumlah pantulan lemah spektroskopi
(ATR/FTIR) menunjukkan bahawa hampir semua lignin dan hemiselulosa telah
dikeluarkan semasa rawatan alkali dan pelunturan. Kajian morfologi terhadap
hierarki gentian telah dijalankan menggunakan mikroskop electron pengimbas
(SEM) dan mikroskop electron transmisi (TEM). X-Ray pembelauan (XRD) pula
menunjukkan bahawa kristaliniti fiber meningkat dari 62.9-81.5% selepas setiap
rawatan yang digunakan. Perbandingan dengan rawatan yang lain menunjukkan
keberkesanan dan hasil melebihi 62.5% bagi nanofibers luntur dan 58% untuk
nanofiber terluntur, dalam pendekatan yang digunakan untuk penghasilan nano
sellulose dari kenaf fiber. Hasil daripada rawatan ini nano fiber yang terpencil
menunjukkan peningkatan kira-kira 10% dalam kestabilan terma berbanding
dengan kenaf fiber yang mentah. Keputusan kajian terhadap sifat luntur terpencil
dan nanofibers luntur menunjukkan lebihan kemungkinan proses pelunturan
sebagai tidak ada kesan yang diperhatikan dalam ciri-ciri mereka.
Walaubagaimanapun, sifat kimia permukaan yang diperoleh daripada gentian
nano yang tidak dilunturkan adalah berbeza dan ia mungkin disebabkan oleh
perlakuan yang berbeza apabila digabungkan kedalam matrik polimer. Dalam
usaha untuk menilai kedua-dua jenis gentian nano yang telah digunakan bagi
memperkukuh matrik kanji termoplastik dan sifat-sifat filem gentian nano, ia telah
dianalisis menggunakan eksperimen SEM, ATR/FTIR, XRD, TGA, kekuatan
tarik, dan penyerapan air. Menariknya, keputusan yang diperoleh oleh filem
komposit nano yang diperbuat daripada gentian nano tidak luntur menunjukkan
prestasi yang lebih baik secara keseluruhannya. Ini adalah hasil kajian yang
bernilai tinggi dan menghapuskan prosedur pelunturan yang berlebihan dalam
proses-proses pengasingan gentian nano.
Dalam usaha untuk membangunkan nano komposit selulosa berasaskan kanji,
gentian nano yang tidak dilunturkan dengan kandungan berlainan (0-10 wt %)
dicampurkan ke dalam matrik kanji termoplastik. Filem bionanokomposit nipis
telah dihasilkan dengan meletakkan dan meruap campuran gentian nanoterampai,
kanji, dangliserol melalui proses pengelatinan dalam masa yang sama. Dalam
usaha untuk menerangkan kepentingan dan kesan gentian selulosa berskalanano,
filem komposit berasaskan kanji dengan keadaan yang sama telah dihasilkan
dengan menggunakan gentian kulit kenaf yang telah dikisar bersaiz mikro.
Komposit dan filem nanokomposit yang terhasil kemudiannya dicirikan
menggunakan eksperimen SEM, TEM, ATR/FTIR, XRD, TGA, DSC, DMTA,
kekuatan tarik, dan penyerapan air. Keputusan yang diperoleh menunjukkan
bahawa antara bahan yang diuji, komposit nano diperkukuh mempunyai sifat yang
lebih baik secara ketara, khususnya; meningkatkan kekuatan mekanikal dan
mengurangkan kepekaan terhadap air. Kekuatan tegangan dan modulus kecil
meningkat sebanyak 313% dan 343% dan penggunaan air dikurangkan sebanyak
21% dengan tambahan sebanyak 10% nanofibers.Hasil kajian menunjukkan
gentian nano gunaan saling bertindak balas secara kuat terhadap ikatan hydrogen
dengan matrik kanji, dan menunjukkan kesesuaian yang disebabkan oleh
persamaan kimia.
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ACKNOWLEDGEMENTS
It is a pleasure to thank the people who made this thesis possible. First of all, I
would like to express my deepest sense of gratitude to my supervisory committee.
Without their help I would not have had the opportunity to work on such a
challenging and valuable project. Many thanks are expressed to Professor Paridah
Md. Tahir for her patience, encouragement and continuous support throughout
this study. Special thanks go to Professor Alain Dufresne for his invaluable
comments, recommendations, kindness and contribution. I am sincerely grateful
for the support and positive attitude of Professor Luqman Chuah Abdullah. I
would like to thank Dr. Ali Abdulkhani who gave me a significant help in
completing this work. I am also grateful to Professor Ali Karimi for his faithful
support and encouragements.
Lots and lots of thanks to all the members of the Institute of Tropical Forestry and
Forest Products, Universiti Putra Malaysia, including staffs and students.
Thanks to dear examiners, which I do not know them, but I want to send my lots
and lots of thanks and respects, for their invaluable time that they allocate to
evaluate this research.
I have spent nice moments in my second country, Malaysia, country of people
from different cultures and religions who live together in peace.
Thanks are also extended to Amirhossein Mehbodnia, Ali Hosseini, Mehdi
Hosseini, and Amin Parvizi. They were there for me during good and bad times,
offering helping hands and being a source of happiness.
I wish to thank my dear brothers, Arash & Afshin, and my sister in-law, Maryam,
for their kindness and support during these years.
Many thanks go to my in-law family for their kindness and prayers, particularly
my dear brother in-law, Mehrdad, for his sincere assistance and online support.
I would like to express my gratitude for the most wonderful part of my life, my
beloved husband, Mehdi, for his unconditional love, encouragement and positive
attitudes.
Last but not the least, I must give very special thanks to my dear uncle and parents
who have taught me to succeed, and for their constant love, patience, calmness,
encouragement and believing me in all these years.
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I certify that a Thesis Examination Committee has met on 24th
January 2014 to
conduct the final examination of Samane Karimimazraehshahi on her thesis
entitled “Characterization of Nanocomposites Based on Plasticized Starch and
Kenaf Bast Nanofibers” in accordance with the Universities and University
Colleges Act 1971 and the Constitution of the Universiti Putra Malaysia [P.U.(A)
106] 15 March 1998. The Committee recommends that the student be awarded the
Doctor of Philosophy.
Members of the Thesis Examination Committee were as follows:
Mohd Sapuan Bin Salit, PhD
Professor
Faculty of Engineering
Universiti Putra Malaysia
(Chairman)
Azmi Zakaria, PhD
Professor
Faculty of Science
Universiti Putra Malaysia
(Internal Examiner)
Azowa Nor Ibrahim, PhD
Doctor
Faculty of Science
Universiti Putra Malaysia
(Internal Examiner)
Martin Hubbe, PhD
Professor
Faculty of Natural Resources
North Carolina State University
United States of America
(External Examiner)
_________________________________
NORITAH OMAR, PhD Associate Professor and Deputy Dean
School of Graduate Studies
Universiti Putra Malaysia
Date: 10 March 2014
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This thesis was submitted to the Senate of Universiti Putra Malaysia and has been
accepted as fulfilment of the requirement for the degree of Doctor of Philosophy.
The members of the Supervisory Committee were as follows:
Paridah Md. Tahir, PhD
Professor
Institute of Tropical Forestry and Forest Products
Universiti Putra Malaysia
(Chairman)
Luqman Chuah Abdullah, PhD
Professor
Faculty of Engineering
Universiti Putra Malaysia
(Member)
Alain Dufresne, PhD
Professor
The International School of Paper, Print Media and Biomaterials
Grenoble Institute of Technology, France
(Member)
Ali Abdulkhani, PhD
Assistant Professor
Faculty of Natural Resources
University of Tehran, Iran
(Member)
_________________________________
BUJANG BIN KIM HUAT, PhD Professor and Dean
School of Graduate Studies
Universiti Putra Malaysia
Date: 3 April 2014
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DECLARATION
Declaration by graduate student
I hereby confirm that:
this thesis is my original work;
quotations, illustrations and citations have been duly referenced;
this thesis has not been submitted previously or concurrently for any other
degree at any other institutions;
intellectual property from the thesis and copyright of thesis are fully-
owned by Universiti Putra Malaysia, as according to the Universiti Putra
Malaysia (Research) Rules 2012;
written permission must be obtained from supervisor and the office of
Deputy Vice-Chancellor (Research and Innovation) before thesis is
published (in the form of written, printed or in electronic form) including
books, journals, modules, proceedings, popular writings, seminar papers,
manuscripts, posters, reports, lecture notes, learning modules or any other
materials as stated in the Universiti Putra Malaysia (Research) Rules 2012;
there is no plagiarism or data falsification/fabrication in the thesis, and
scholarly integrity is upheld as according to the Universiti Putra Malaysia
(Graduate Studies) Rules 2003 (Revision 2012-2013) and the Universiti
Putra Malaysia (Research) Rules 2012. The thesis has undergone
plagiarism detection software.
Signature: _______________________ Date: 24 January 2014
Name and Matric No.: Samaneh Karimimazraehshahi (GS24934)
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Declaration by members of supervisory committee
This is to confirm that:
the research conducted and the writing of this thesis was under our
supervision;
supervision responsibilities as stated in the Universiti Putra Malaysia
(Graduate Studies) Rules 2003 (Revision 2012-2013) are adhered to.
Signature: __________________
Name of
Chairman of
Supervisory
Committee: Paridah Md. Tahir, PhD
Signature: __________________
Name of
Member of
Supervisory
Committee: Alain Dufresne, PhD
Signature: __________________
Name of
Member of
Supervisory
Committee: Luqman Chuah Abdullah, PhD
Signature: __________________
Name of
Member of
Supervisory
Committee: Ali Abdulkhani, PhD
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TABLE OF CONTENTS
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ACKNOWLEDGEMENTS vii
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3 PREPARATION OF NANOFIBERS FROM KENAF BAST Error!
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4 PROPERTIES OF STARCH BASEDBIONANOCOMPOSITES MADE
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5 EFFECT OF MICRO AND NANO REINFORCEMENTES ON
MECHANICAL BEHAVIOR OF STARCH BASED COMPOSITES
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6 EFFECT OF MICRO AND NANO REINFORCEMENTES ON
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7 OVERALL CONCLUSIONS AND RECOMMENDATIONS FOR
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