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Nano-Characterization of Ceramic-Metallic Interpenetrating Phase Composite Material Using Electron Crystallography

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Nano-Characterization of Ceramic-Metallic Interpenetrating Phase Composite Material Using Electron Crystallography YOUNGSTOWN STATE UNIVERSITY Nano-Characterization of Ceramic-Metallic Interpenetrating Phase Composite Material using Electron Crystallography by Marjan Moro Submitted in Partial Fulfillment of the Requirements for the Degree of Master of Science in Engineering in the Mechanical Engineering Program Mechanical and Industrial Engineering May 2012 Nano-Characterization of Ceramic-Metallic Interpenetrating Phase Composite Material using Electron Crystallography by Marjan Moro I hereby release this thesis to the public. I understand that this thesis will be made available from the OhioLINK ETD Center and the Maag Library Circulation Desk for public access. I also authorize the University or other individuals to make copies of this thesis as needed for scholarly research. Signature: Marjan Moro, Student Date Approvals: Dr. Virgil C. Solomon, Thesis Advisor Date Dr. Matthias Zeller, Committee Member Date Dr. Timothy R. Wagner, Committee Member Date Dr. Hyun W. Kim, Committee Member Date Dr. Peter J. Kasvinsky, Dean of Graduate Studies Date i Abstract Interpenetrating phase composites (IPCs) have unique mechanical and physical proper- ties and thanks to these they could replace traditional single phase materials in numbers of applications. The most common IPCs are ceramic-metallic systems in which a duc- tile metal supports a hard ceramic making it an excellent composite material. Fireline, Inc., from Youngstown, OH manufactures such IPCs using an Al alloy-Al2O3 based ceramic-metallic composite material. This product is fabricated using a Reactive Metal Penetration (RMP) process to form two interconnected networks. Fireline products are used, among others, as refractory materials for handling of high temperature molten metals. A novel route to adding a shape memory metal phase within a ceramic matrix has been proposed. A NiO preform was reacted with Ti to produce an IPC using a plasma arc melting system. This reaction is particularly interesting due to the possible formation of a Ni-Ti metal phase which could exhibit shape memory effects within the ceramic-metal network. Different ratios of NiO and TiO2 (rutile) were reacted with Ti to investigate if the NiTi phase could be formed. In this thesis, two IPCs, one produced by the TCON RMP process and the other by using plasma arc-melting were investigated. The materials include Al-Fe alloy-Al2O3 and NiO-Ti ceramic-metallic IPCs. Analysis was performed using scanning/transmission electron microscopy (S/TEM), energy dispersive spectroscopy (EDS), focused ion beam (FIB), and X-ray diffraction (XRD). Observations of these IPCs revealed all present phases within the composite material, obtained orientation relationships, and explored the growth mechanism of the RMP process which still puzzles the scientific community. This information is valuable for developing improved IPC systems with diverse elemental composition for a wide variety of applications. Acknowledgements I want to thank my family for the love and support they have provided to me throughout my schooling. I would like to thank my advisor, Dr. Virgil Solomon, for constantly challenging me to achieve more while guiding me in the right direction during my graduate studies at Youngstown State University. The expertise he has shared with me will certainly help me in my professional career. Furthermore, working with Dr .Solomon has helped me grow as an individual. I would also like to thank my thesis committee members. First and foremost I would like to thank Dr. Matthias Zeller for spending endless amount of time with me having fruitful discussions. Next I would like to thank Dr. Timothy Wagner for allowing me to use his lab space and for managing my student funding during my studies. Lastly, I would like to thank Dr. Hyun Kim for being there from the beginning to end of my graduate studies and guiding me through the graduate school process. I am also appreciative of Mr. Klaus-Markus Peters and Mr. Brian Hetzel of Fireline Inc. for providing me with the opportunity to study their company’s products. Finally, I would like to thank my friends and family for listening to me talk hours upon hours about all the academics that I enjoy so much and for trying to understand what captivates me. iii Contents Abstract ii Acknowledgements iii List of Figures vi List of Tables viii List of Symbols and Terminology ix 1 Introduction1 2 Background6 2.1 Introduction to Interpenetrating Phase Composites (IPCs).........6 2.2 Chronological Literature Review on IPCs..................7 2.3 Modus Operandi of Ceramic-Metallic IPCs................. 16 2.3.1 Conditions for IPCs.......................... 16 2.3.2 Transformation mechanism...................... 17 2.4 Alumina-Aluminum System.......................... 19 2.4.1 TCON/RMP Process......................... 19 2.4.2 Fe-Additives to the Al2O3/Al system................. 20 2.4.3 Alloying Aluminum with Iron and Silicon.............. 22 2.4.4 Previously Obtained Results..................... 23 2.5 Nickel Oxide-Titanium System........................ 27 2.5.1 Literature................................ 28 2.5.2 Shape Memory Alloys......................... 30 3 Experimental 36 3.1 Sample Acquisition and Sample Preparation................. 36 3.1.1 TCON Material............................ 36 3.1.2 NiO-Ti System............................. 37 3.2 Instrumentation................................. 41 iv Contents v 3.2.1 Transmission Electron Microscopy.................. 41 3.3 Electron Crystallography........................... 45 3.3.1 Selected Area Diffraction Patterns and jEMS Software....... 48 3.4 High Resolution Electron Microscopy..................... 51 3.4.1 Multislice Method........................... 52 4 Results 54 4.1 TCON Material................................. 54 4.1.1 Introduction.............................. 54 4.1.2 Preliminary Analysis.......................... 54 4.1.3 Phase identification by Electron Crystallography.......... 56 4.1.4 Orientation Relationships....................... 65 4.1.5 Silicon Inclusions............................ 71 4.1.6 HREM Investigations......................... 77 4.2 NiO-Ti Results................................. 83 4.2.1 Trial Run 1............................... 83 4.2.2 Trial Run 2............................... 91 4.2.3 Trial Run 3............................... 92 4.2.4 NiO-TiO Pellet Trials......................... 92 5 Conclusion 95 5.1 Fireline Material................................ 95 5.2 NiO-Ti material................................. 97 6 References 99 A Python Script 107 B Camara Length 109 List of Figures 2.1 Breslin’s Mechanism.............................. 18 2.2 Binary Fe-Al Phase Diagram......................... 22 2.3 Ternary Al-Fe-Si Phase Diagram....................... 23 2.4 Powder XRD of TCON Material....................... 24 2.5 EDS analysis of TCON Material....................... 25 2.6 Gibbs Free Energy Diagram of Possbile Sacrificial Oxdies......... 29 2.7 Shape Memory Effect via Temperature.................... 32 2.8 Shape Memory Alloys Superelasticity..................... 33 2.9 The Nickel-Titanium Phase Diagram..................... 34 3.1 NiO Pellet XRD................................ 37 3.2 Ti XRD..................................... 38 3.3 NiO Pellet Process............................... 39 3.4 TEM Ray Diagram............................... 43 3.5 Beam Specimen Interaction.......................... 44 3.6 Bravais Lattice................................. 47 3.7 Typical Diffraction Pattern.......................... 49 3.8 jEMS Procedure................................ 50 3.9 Transfer Function................................ 52 3.10 Multislice Illustration............................. 53 4.1 Backscatter Electron Micrograph and EDS Elemental Map of Sample... 55 4.2 Al2O3 and Al;EDS and SADP......................... 56 4.3 Manual Indexing................................ 57 4.4 Result of Manual Indexing........................... 60 4.5 Ternary Phase Analysis............................ 62 4.6 Binary Phase Analysis............................. 64 4.7 Binary Phase Analysis............................. 66 4.8 Orientation Relationship Atomic Model between Al2O3 and Al...... 67 4.9 Orientation Relationship betweem Al2O3 and Al13Fe4 ........... 68 4.10 Orientation Relationship Atomic Model between Al13Fe4 and Al2O3 ... 69 4.11 Orientation Relationship betweem Al2O3 and Al13Fe4 ........... 70 4.12 Typical Silicon Inclusions........................... 71 4.13 Darkfield and Brightfield Images of Silicon Inclusions........... 72 4.14 Modulation in Silicon............................. 74 vi List of Figures vii 4.15 High Resolution Images of Silicon Inclusion................. 75 4.16 High Resoltuion Image from Al2O3 and the Al-Fe Boundary........ 79 4.17 High Resoltuion Image from Alumina.................... 80 4.18 Map of Thickness and De-focus........................ 81 4.19 Rresults of Multislice Simulation....................... 82 4.20 Macroscopic View of NiO-Ti Sample..................... 84 4.21 Light Microscope Analysis of NiO-Ti Sample................ 85 4.22 NiO-Ti XRD.................................. 86 4.23 NiO-Ti SEM Analysis............................. 87 4.24 NiO-Ti SEM Analysis............................. 88 4.25 NiO-Ti SEM Analysis............................. 89 4.26 Backscatter Electron Micrograph of NiO-Ti Sample............. 89 4.27 NiO-Ti SEM and EDS Analysis........................ 90 4.28 NiO-Ti Backscatter Electron Image and EDS Elemental Map....... 90 4.29 50wt.%NiO-50wt.% Ti pellrts results..................... 93
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