UNIVERSITI PUTRA MALAYSIA IMPREGNATION OF IN-HOUSE SYNTHESIZED CARBON NANOTUBES INBACTERIAL CELLULOSE

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1 UNIVERSITI PUTRA MALAYSIA IMPREGNATION OF IN-HOUSE SYNTHESIZED CARBON NANOTUBES INBACTERIAL CELLULOSE SHARMEEN BINTI ADNAN FK

2 IMPREGNATION OF IN-HOUSE SYNTHESIZED CARBON NANOTUBES IN BACTERIAL CELLULOSE By SHARMEEN BINTI ADNAN Thesis Submitted to the School of Graduated Studies, Universiti Putra Malaysia, in Fulfillment of the Requirement for the Degree of Master of Science August 2011

3 Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfillment of the requirement for the degree of Master of Science. IMPREGNATION OF IN-HOUSE SYNTHESIZED CARBON NANOTUBES IN BACTERIAL CELLULOSE Chair: Dayang Radiah Bt. Awang Biak, PhD Faculty: Faculty of Engineering By SHARMEEN BINTI ADNAN August 2011 Bacterial cellulose (BC) synthesized by Acetobacter xylinum has been discovered as a potential matrix for impregnating carbon nanotubes (CNT). The main objective of this study is to produce bacterial cellulose/carbon nanotube (BC/CNT) with improved hydrophobic surface. CNT addition is by mean to improve the electrical property of BC to be a conductive membrane. Hydrophobic membrane is more practical in device development since it can adhere with other hydrophobic material, which is achieved in this study by acetylation process. In this work, the membranes were produced using date extract (DE) culture medium. Three CNT impregnation techniques were tested, i.e. immersion, dispersion and spraying, whilst the acetylation conducted were homogeneous and heterogeneous processes. ii

4 In this study, morphological characteristic is an important property for sample selection to be characterized further. BC/CNT nanocomposite produced via spraying technique has uniform CNT dispersion and has the most dielectric conductivity value i.e. ~4.66 x 10-1 S/cm than the other techniques. Therefore, spraying was used to prepare BC/CNT acetate nanocomposite. Since the morphology of BC/CNT acetate obtained from heterogeneous process proves that the acetylation only occurred on the surface and the inner core structures of the BC are still intact, this process was used further. The most significant characteristic of BC/CNT acetate is the existence of C=O, CH 3 and C-O functional groups of acetyl and higher water contact angle (~77 ) than that of BC/CNT (~45 ). When tested, decomposition and glass transition temperatures of BC/CNT acetate have reduced by 203 C and 35 C respectively, compared to that BC/CNT. The reduction is occurred mainly because the swollen BC structure of BC/CNT acetate is easily degraded by heat treatment. The acetylated BC/CNT on the other hand, has higher crystal BC fraction, i.e. 51% compared to that of BC/CNT (49%). These findings indicate that the CNT hinders the degradation of nanocomposite and protects the BC crystals. Thus when acetylated, both elasticity and crystallite size of BC/CNT has only reduced by 9%, i.e., from 34 to 31 GPa and from 27.3 to 24.9 nm, respectively. The bigger pore size of the acetate nanocomposite (~22 Å) than that of BC/CNT (~-103 Å) might allows further functionalization process introduced to the membrane. As a conclusion, the CNT impregnation by spraying technique during the growing fermentation of BC coupled with heterogeneous acetylation treatment resulted in a more water resistant, iii

5 increased dielectric conductivity and increased crystal BC fraction. While, the sheet elasticity, crystallite size, surface area, decomposition and glass transition temperatures became lower. These characteristics makes acetylated BC/CNT sheet a potential as a biomaterial membrane in device development. iv

6 Abstrak tesis yang dikemukan kepada Senat Universiti Putra Malaysia sebagai memenuhi keperluan untuk Ijazah Master Sains. IMPREGNASI NANOTIUB KARBON YANG DISINTESIS SECARA DALAMAN KE DALAM SELULOSA BAKTERIA Oleh SHARMEEN BINTI ADNAN Ogos 2011 Pengerusi: Dayang Radiah Bt. Awang Biak, PhD Fakulti: Fakulti Kejuruteraan Selulosa bakteria (BC) yang disintesis oleh Acetobacter xylinum telah dikenalpasti sebagai matriks yang berpotensi tinggi untuk diisi dengan nanotiub karbon (CNT). Objektif utama penyelidikan ini adalah untuk menghasilkan nano-komposit selulosa bakteria/nanotiub karbon (BC/CNT) dengan permukaan hidrofobik. CNT ditambahkan bagi memperbaiki ciri elektrikal BC seterusnya menghasilkan membran yang konduktif. Membran yang hidrofobik pula lebih praktikal dalam penghasilan peralatan kerana ia lebih sesuai untuk digunakan bersama bahan hidrofobik yang lain. Dalam penyelidikan ini, membran dihasilkan menggunakan media kultur daripada ekstrak kurma. Tiga teknik impregnasi CNT yang dijalankan adalah rendaman, v

7 serakan dan semburan manakala proses asetilasi pula adalah proses asitilasi penuh dan asitilasi separa. Dalam kajian ini, morfologi adalah ciri penting dalam pemilihan sampel yang akan dianalisa sepenuhnya. Nano-komposit BC/CNT yang dihasilkan melalui teknik semburan menunjukkan keseragaman penyebaran CNT serta mempunyai nilai konduktiviti di-elektrik yang paling baik iaitu ~4.66x 10-1 S/cm berbanding nilai yang ditunjukkan oleh BC/CNT yang dihasilkan melalui teknik-teknik yang lain. Maka, teknik semburan telah digunakan untuk menghasilkan nanokomposit BC/CNT asetat. Disebabkan morfologi BC/CNT asetat yang disediakan melalui proses asitilasi separa menunjukkan degradasi hanya berlaku di permukaan sahaja sementara struktur teras dalam BC tidak terjejas, maka proses ini digunakan untuk penghasilan sampel seterusnya. Ciri BC/CNT asetat dikenalpasti melalui kewujudan ikatan-ikatan yang mewakili kumpulan berfungsi asetil iaitu C=O, CH 3 dan C-O dan juga nilai sudut antara air dan BC/CNT asetat yang lebih tinggi (~77 ) berbanding BC/CNT (~45 ). Apabila kedua-duanya dikaji, suhu penguraian dan peralihan kaca bagi BC/CNT asetat menurun kepada 203 C dan 35 C, masingmasing. Penurunan ini berlaku kerana struktur BC dalam BC/CNT asetat yang membengkak memudahkannya diuraikan dengan rawatan suhu. vi

8 Namun begitu, BC/CNT asetat mempunyai kandungan hablur BC yang lebih tinggi, iaitu 51% berbanding BC/CNT (49%). Ini menunjukkan CNT telah menghalang proses penguraian nanokomposit seterusnya melindungi hablur BC. Disebabkan itu, kedua-dua keupayaan elastik dan saiz hablur BC/CNT hanya menurun sebanyak 9% sahaja, iaitu daripada 34 ke 31 GPa dan daripada 27.3 ke 24.9 nm, masing-masing. Tambahan pula, liang nano-komposit asetat yang lebih besar (~22 Å) berbanding BC/CNT (~-103 Å) mungkin membolehkan proses penambahbaikan fungsi dilakukan ke atas membran tersebut. Kesimpulannya, impregnasi CNT melalui teknik semburan semasa fermentasi BC berlaku disamping rawatan asetilasi separa telah menghasilkan membran yang rintang kepada air, tinggi nilai konduktiviti dielektrik dan tinggi kandungan hablur BCnya. Namun, keupayaan elastik, saiz hablur, suhu penguraian dan suhu peralihan kaca telah menurun. Ciri-ciri ini menjadikan membran BC/CNT asetat berpotensi sebagai biomaterial membran dalam pembuatan peralatan. vii

9 ACKNOWLEDGEMENT In the name of Allah S.W.T., the most Benevolent and Merciful. All gratification is referred to Allah S.W.T. Firstly, I would like to take this opportunity to thank the chairperson of my supervisory committee, Dr. Dayang Radiah Bt. Awang Biak, whose expert guidance and support has helped me to complete the research. Her kindness, affection, encouragement and moral support gave me the courage and ability to overcome all the problems I have faced from time to time during the course of my work. I would like to extend my appreciation to her for the invaluable advice and continuous comment and support, which brighten my future through the experiences that I have gained from her. I am also very grateful to Mrs. Faizah Bt. Md. Yasin, whose expert guidance and support has helped me to overcome problems that I have encountered during the course of my study. I am also indebted to and wish express my appreciation to Mrs. Suryani Bt. Kamaruddin for her interest and invaluable suggestion that had enable me to carry on with my project successfully. viii

10 I would like to thank Universiti Putra Malaysia for providing me a scholarship (Graduate Research Fellowship) which has enables me to continue my research as well as my life a student. The list of thanks also goes to all my friends and the people who have known me for the joy, laughter and memories that we have shared together during my study at Universiti Putra Malaysia. Lastly, I would like to express my most sincere and warmest gratitude to my mother (Siti Hafsah Bt. Dahalan) and my father (Adnan B. Rajikan) and all my family members for their payers, love, generosity and moral supports that they have during the course of my study. ix

11 I certify that a Thesis Examination Committee has met on 25 August 2011 to conduct the final examination of Sharmeen Binti Adnan on her thesis entitled "Impregnation of In-House Synthesized Carbon Nanotubes in Bacterial Cellulose" in accordance with the Universities and University Colleges Act 1971 and the Constitution of the Universiti Putra Malaysia [P.U.(A) 106] 15 March The Committee recommends that the student be awarded the degree of Master of Science. Members of the Thesis Examination Committee were as follows: Fakhru l-razi Ahmadun, PhD Professor Dr. Faculty of Engineering Universiti Putra Malaysia (Chairman) Robiah Yunus, PhD Professor Dr. Faculty of Engineering Universiti Putra Malaysia (Internal Examiner) Suraya Abdul Rashid, PhD Dr. Faculty of Engineering Universiti Putra Malaysia (Internal Examiner) Fadzilah Adibah Abdul Majid, PhD Associate Professor Dr. Department of Bioprocess Engineering, Faculty of Chemical Engineering Universiti Teknologi Malaysia Malaysia (External Examiner) SEOW HENG FONG, PhD Professor and Deputy Dean School of Graduate Studies Universiti Putra Malaysia Date: 20 December 2011 x

12 This thesis was submitted to the Senate of Universiti Putra Malaysia and has been accepted as fulfillment of the requirement for the degree of Master of Science. The members of the Supervisory Committee were as follows: Dayang Radiah Bt. Awang Biak, PhD Senior Lecturer Faculty of Engineering Universiti Putra Malaysia. (Chairman) Faizah Bt. Md. Yasin Lecturer Faculty of Engineering Universiti Putra Malaysia. (Member) BUJANG BIN KIM HUAT, PhD Professor and Dean School of Graduate Studies Universiti Putra Malaysia Date: xi

13 DECLARATION I declare that the thesis is my original work except for quotations and citations which have been duly acknowledged. I also declare that it has not been previously, and is not concurrently, submitted for any other degree at Universiti Putra Malaysia or at any other institution. SHARMEEN BINTI ADNAN Date: 25 August 2011 xii

14 TABLE OF CONTENTS ABSTRACT ABSTRAK ACKNOWLEDGEMENT APPROVAL DECLARATION LIST OF TABLES LIST OF FIGURES LIST OF ABBREVIATIONS CHAPTER 1. INTRODUCTION 1 2. LITERATURE REVIEW Introduction Bacterial cellulose (BC) Growth associate product of BC Carbon source as crucial nutrient Oxygen dependent of BC production Crystal structure of BC microfibrils BC nanocomposites Carbon nanotubes (CNT) and bacterial cellulose/ 20 carbon nanotubes (BC/CNT) nanocomposites Previous researches on BC/CNT nanocomposites Dielectric properties of BC/CNT nanocomposites Acetylation of BC and BC/CNT membranes Mechanism of acetylation Methodology of acetylation Characterization of BC and BC/CNT membranes Morphological analysis 29 Page ii v viii x xii xvii xviii xxi xiii

15 2.4.2 Spectroscopic identification Thermal characteristic Mechanical characteristic Surface analysis Wettability Surface area and porosity Conclusion METHODOLOGY Introduction Preparation of date extract (DE) Culture medium preparation from DE Production of BC membrane Recovery process of BC membrane Sample preparation for characterization Experiment for carbon source selection Production of BC/CNT membrane (A) Immersing BC membrane in CNT 41 dispersed solution (B) Dispersing CNT in DE culture medium (C) Spraying CNT dispersed solution onto growing BC 42 (a) Preparation of DE culture medium and 42 CNT dispersed solution (b) Spraying procedure of CNT dispersed solution Dielectric conductivity calculation of BC/CNT membranes Preparation of BC/CNT acetate nanocomposite Homogeneous acetylation Heterogeneous acetylation Characterization of BC and nanocomposite membranes Morphological observation Spectroscopic identification 47 xiv

16 Crystallinity analysis Thermal analysis Mechanical analysis Surface wettability analysis Surface area and porosity analysis Conclusion RESULTS AND DISCUSSION Introduction Comparison of the BC produced from HS and DE media Production of BC/CNT nanocomposites CNT dispersion behavior within BC membrane 58 (A) Immersing BC membrane in CNT 59 dispersed solution (B) Dispersing CNT in BC culture medium 60 (C) Spraying CNT dispersed solution 62 onto growing BC Physical characteristic of BC/CNT nanocomposites Dielectric conductivity of the produced BC/CNT Production of BC/CNT acetate nanocomposite Physical changes of BC and BC/CNT due to acetylation 70 (A) Homogeneous acetylation 71 (B) Heterogeneous acetylation Morphological observation Character of BC produced using DE culture medium Character of BC/CNT nanocomposites 75 (A) Immersing BC membrane in CNT 75 dispersed solution (B) Dispersing CNT in DE culture medium 76 (C) Spraying CNT dispersed solution onto growing BC Morphological changes of BC and BC/CNT acetates 79 xv

17 4.5 Spectroscopic identification The significant functional groups of the membranes Determination of cellulose crystals via FTIR analysis Crystallinity analysis Crystalline peaks of the membranes Determination of crystallite size Determination of crystallinity index (CrI) Thermal analysis Weight loss percentage of the membranes Determination of decomposition temperature Mechanical analysis Elasticity of the membranes Viscous dissipation of the membranes Determination of glass transition temperature (T g ) Surface wettability analysis Surface area and porosity analysis Pore size investigation Determination of surface area Conclusion SUMMARY, CONCLUSION AND 113 RECOMMENDATIONS FOR FUTURE RESEARCH REFERENCES 117 APPENDICES 130 BIODATA OF STUDENT 136 xvi

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