Haider master's thesis

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this My thesis about TiO2 Nanotube

Text of Haider master's thesis

  • 1. Fabrication of TiO2 Nanotubes Using Electrochemical AnodizationRepublic of Iraq Ministry of Higher Education and Scientific Research University of BaghdadCollege of Science Fabrication of TiO2 Nanotubes UsingElectrochemical AnodizationA Thesis Submitted to the University of Baghdad, College of Sciences, Department of Physics asa Partial Fulfillment of the Requirements for the Degree of Master of Science in Physics By Haidar H. Hamdan Al-Eqaby B.Sc., Al Mustansiriyah University, 2007Supervised byProf. Dr. Harith I. JaafarLect. Dr. Abdulkareem M. Ali 2012 AD1433 AH1

2. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization( ) 582 3. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization DEDICATIONTo:My mother My father My BrothersMy SistersMy Uncle Mr. JabbarMy close friendsMy country beloved IraqThe martyrs of Iraq with all the love and appreciation. Haidar3 4. Fabrication of TiO2 Nanotubes Using Electrochemical AnodizationACKNOWLEDGEMENTSPraise be to ALLAH, his majesty for his uncountable blessings, and bestprayers and peace be unto his best messenger Mohammed, his pure descendant,and his family and his noble companions.First I would like to thank my family. Without their love and support overthe years none of this would have been possible. They have always been therefor me and I am thankful for everything they have helped me achieve.Next, I would like to thank my supervisors Prof. Dr. Harith I. Jaafarand lect. Dr. Abdulkareem M. Ali, Dr. Harith your help and guidance over theyears which is unmeasurable and without it I would not be where I am today.Dr. Harith, what can I say, as graduate students we are truly fortunate to haveyou in the department. I thank you so much for the knowledge you have passedon and I will always be grateful for having the opportunity to study under you. Iwould like to thank Dr. Kamal H. Lateif, Dr. Baha T. Chiad, Dr. Shafiq S.Shafiq, Dr. Fadhil I. Shrrad, Dr. Kadhim A. Aadim, Dr. Issam, Dr. Sadeem,Dr. Qahtan, Dr. Muhammad K., Mr. Muhammad U., Mr. Issam Q., Mr.Muhammad J., Ms. Duaa A. and Ms. Hanaa J. for their assistance. This workwould not have been possible without their help and input.I would also like to express my thanks to the deanery of the College ofSciences and head of Physics Department for their support ship to the student ofhigher education, the faculty is irreplaceable and their generosity to the studentbody is incomparable.Thank to Prof. Dr. Moohajiry (Tehran University) and his researchgroup to provide me an Opportunity to work in his respectable laboratory (SEMTechnician). 4 5. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization To my fellow graduate students, thank you for the good times throughoutour years. Whether it was late nights studying or in the University, it was alwaysa good time. I wish everyone good luck in the future and hope our paths crossagain. In addition, I would like to thank my friends from Al-MustansiriyaUniversity, especially the Assistant Lecturer Ms. Marwa A. Hassan. Fromthe times that escalated quickly to showing me the way to victory lane, itseems like weve never missed a beat. Finally I would like to thank all of the other friends that I developed overthe years. I am a lucky person to have the friendships that I have. Haidar5 6. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization Supervisor Certification We certify that this thesis titled Fabrication of TiO2 Nanotube UsingElectrochemical Anodization was prepared by Mr. (Haidar H. Hamdan),under our supervision at Department of Physics, College of Science, Universityof Baghdad, as a partial fulfillment of the requirements for the degree of Masterof Science in Physics.Signature: Signature: (Supervisor)(Supervisor)Name: Dr. Harith I. Jaafar Name: Dr. Abdulkareem M. AliTitle: Professor Title: LecturerDate: 5 / 3 / 2012 Date: 5 / 3 / 2012In view of the available recommendation, I forward this thesis for debateby the Examination Committee.Signature:Name: Dr. Raad M.S AL- HaddadTitle: ProfessorAddress: Head of Physics Department,Collage of Science, University of Baghdad.Date: 5 / 3 / 20126 7. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization Examination Committee Certification We certify that we have read this thesis entitled Fabrication of TiO2Nanotube Using Electrochemical Anodization as an examine committee,examined the student Mr. (Haidar Hameed Hamdan) in its contents and that,in our opinion meets the standard of thesis for the degree of Master of Science inPhysics.Signature:Signature:Name: Dr. Ikram A. Ajaj Name: Dr. Raad S. SabryTitle: Assistant ProfessorTitle: Assistant ProfessorAddress: University of BaghdadAddress: Al-Mustansiriyah UniversityDate: 25 / 4 /2012Date: 25 / 4 /2012(Chairman)(Member)Signature:Signature:Name: Dr. Inaam M. AbdulmajeedName: Dr. Dr. Harith I. JaafarTitle: Assistant ProfessorTitle: ProfessorAddress: University of Baghdad Address: University of BaghdadDate: 25 / 4 /2012Date: 25 / 4 /2012(Member)(Supervisor)Signature:Name: Dr. Abdulkareem M. Ali Title: Lecturer Address: University of Baghdad Date: 25 / 4 /2012 (Supervisor)Approved by the Council of the College of Science.Signature:Name: Dr. Saleh M. AliTitle: ProfessorAddress: Dean of the Science College,University of BaghdadDate: 27 / 4 /2012 7 8. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization AbstractThis thesis describes the synthesis of self-organized titanium dioxidenanotube layers by an electrochemical anodization of Ti at differentconditions (time, voltage, concentration of NH4F in electrolyte withglycerol, conductivity and water content) at room temperature (~25C)were investigated.In the current study, self-organized, vertically-oriented TiO2nanotubes were successfully prepared by anodization method of a pureTitanium sheet (99.5%) using anodization cell is designed for first time inIraq (Homemade) from Teflon material according to our knowledge toproduce self-ordered Titanium nanotube in organic based electrolytes(glycerol based electrolyte) an electrolyte solution containing (0.5, 1, 1.5and 2 wt.% NH4F) then added water (2 and 5Wt.% H2O) to (0.5wt.%NH4F) only with 15V. The range of anodizing time and potential werebetween 1-4hr. and 5-40V, where Wt.% represent weight percentage.Scanning electron microscopy (SEM), Atomic force microscopy(AFM) and (XRD) X-Ray diffraction were employed to characterize themorphology and structure of the obtained Titania templates, opticalinterferometer (Fizeau frings) method to tubes length measurement.For TiO2 nanotubes fabricated in non-aqueous electrolyte, theinfluence of the NH4F concentration on characteristics of nanotubes wasstudied. The results showed that when the NH4F concentration increasedfrom 0.5 to 2wt.%NH4F, the tubes diameter, tubes length and roughness ofTiO2 surface increased.Also the effects of the anodizing time and anodizing potential werestudied. The formation of TiO 2 nanotubes was very sensitive to the 8 9. Fabrication of TiO2 Nanotubes Using Electrochemical Anodizationanodizingtime. Lengthof the tube increases withincreasing anodizing time and anodizing potential significantly.Either water content (2 and 5wt.%) with 0.5wt.% NH4F and theconductivity of electrolyte it is increasing the diameter, tube length androughness of TiO2 surface increased, but simple increasing and formationof less homogenized TiO2 nanotube.The optimal conditions for TiO2 formation was found 15V at 4hrwith 0.5wt.% NH4F due to we obtain on best results for tube diameter, tubewall thickness, tube length and more homogenized of TiO2 nanotubes. 9 10. Fabrication of TiO2 Nanotubes Using Electrochemical AnodizationContentsTitlePageDedication 3Acknowledgments4Supervisor Certification 6Examination Committee Certification7Abstract 8Contents 10List of Figures13List of Tables 15List of Abbreviation 16Chapter One (Introduction and Literature Review)ParagraphTitle Page1-1Physical and Chemical Science and Nanotechnology191-2Nanomaterials 191-3Types of nano materials 201-4Literature Review 211-5Aim of this Work26Chapter Two (Theoretical Part)ParagraphTitle Page2-1Introduction to Nanotechnology282-2Quantum Confinement in Semiconductors 302-2-1Quantum Dot 302-2-2Quantum Wire302-2-3Quantum Well302-3Summary of Quantum Confinement Effect 312-4Micro to Nano Materials Perspective 322-5Strategies of Making Nanostructures 332-6Properties of Titanium Dioxide (TiO2) 342-6-1Crystal Structure of Titanium Dioxide (TiO2)352-6-1-1Titanium Dioxide (TiO2) in Rutile Stable Phase352-6-1-2Titanium Dioxide (TiO2) in Anatase Metastable Phase 362-6-1-3Titanium Dioxide (TiO2) in Brookite Structure 372-7Synthesis Techniques of TiO2 nanotube 392-8Electrochemical Anodization processes 39 11 11. Fabrication of TiO2 Nanotubes Using Electrochemical Anodization2-9 Electrochemical Anodization of Metals402-10Mechanism of TiO2 nanotubes array formation422-11Factors affecting the formation of (TiO2) nanotube 462-11-1The effect of anodization potential462-11-2The effect of electrolyte472-11-3The effect of temperature482-11-4The effect of annealing before and after anodizing 492-11-5The effect of distance between electrodes49Chapter Three (Experimental and Methods)Paragraph TitlePage3-1 Introduction 523-2 Chemicals and Instrumentations 523-2-1 Chemicals523-2-2 Instrumentations 533-2-3 Processes flow chart of template synthesis 543-3 Electrochemical Anodization system 553-3-1 Electrochemical Anodization Cell Design553-4 Samples preparation563-4-1 Pretreatment of Ti samples 563-4-2 TiO2 Nanotube preparation573-5 Characterization measurements593-5-1 X-Ray diffraction (XRD) pattern593-5-2 Atomic Force Microscopy (AFM)603-5-3 Scanning Electron Microscopy(SEM)613-5-4 Thickness measurement62 Chapter Four (Results and Discussions)Paragraph TitlePage4-1 Introduction 654-2 (I-V) characteristics of the electrochemical 65anodization process4-2-1 Effect of NH4F concentration 654-2-2 Effect of anod