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Deposition Kinetics of Titanium and Zirconium Diffusion Coatings on Nickel Microwires Via Pack Cementation

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Deposition Kinetics of Titanium and Zirconium Diffusion Coatings on Nickel Microwires Via Pack Cementation Deposition Kinetics of Titanium and Zirconium Diffusion Coatings on Nickel Microwires via Pack Cementation A thesis submitted to the Division of Research and Advanced Studies of the University of Cincinnati in partial fulfillment of the requirements for the degree of Master of Science in the program of Materials Science and Engineering in the Department of Mechanical and Materials Engineering of College of Engineering and Applied Science University of Cincinnati, Ohio, USA By Ajith Achuthankutty Committee Members: Dr. Ashley Paz y Puente (Chair) Dr. Matthew Steiner Dr. Sarah Watzman Fall 2019 i ACKNOWLEDGEMENT My grad life, full of ups and downs, could not have been fulfilled without the guidance, support, and cooperation of so many people. Firstly, I thank god almighty for helping me with all the resources in this venture. Next, I am deeply indebted to my mentor and advisor, Dr. Ashley Paz y Puente, for giving me this fantastic opportunity to work in her lab. Her support and continued motivations were the major driving forces during my master’s program at the University of Cincinnati. It was a little difficult for me initially to change track from mechanical to material science, but her consistent encouragement and training made it easy for me to hone my skills. I am also grateful to her for supporting me with Teaching Assistantships, which helped to manage classes, improve my knowledge, presentation, and soft skills. I am really thankful to Dr. Dinc Erdeniz for providing the training and installation of the lab equipment and giving me ideas and guidelines for this research. I would also like to acknowledge Dr. Matthew Steiner and Dr. Sarah Watzman for agreeing to be on my defense panel and supporting my work with valuable suggestions. I thank Dr. Melodie Fickenscher for helping and training me on SEM micrographs, elemental analysis data, and other characterization tools that were prominently used for this thesis work. No words can express my respect and love towards my parents Mrs. Jayasree Nair and Mr. Achuthankutty Nair and my siblings Arun Nair and Neethu Krishna. They were confident enough to send me abroad to achieve my dream and passion. My extreme gratitude to Arathi Anil Sushma for helping through my hard times and motivating me in completing my degree ii and finding a suitable job. She has been a pillar and a great role model to me both academically and otherwise. I am really blessed to have such extremely supporting and helpful lab-mates. I thank Arun Bhattacharjee, Pavan Ajjarapu, Haozhi Zhang and Safa Khodabakhsh for assisting me with my research and giving timely inputs and suggestions. My life at Cincinnati would not have been a memorable one without my friends; Abhishek Pai, Lavanya Varma, Anjaly Vijayan, Madhavan Sudhakar, Ketan Shah, Jose Joseph, Gibin Raju, Smriti Jha, and Anantharaman Ashok. Finally, a special thanks to my classmates Pavan Kandala, Suriya Sekar, Sakshi Satyanarayana and Biswajit Dalai for all the fun-packed times during the course. iii ABSTRACT Pack cementation is a promising technique to synthesize hollow NiTi microtubes, which impart enhanced heating/cooling efficiency and, thus, faster shape memory response. Prior research investigating the effect of wire size on phase evolution and Kirkendall pore formation during pack titanization showed a significant difference between large (100 µm) and small (25 µm) diameter wires. The first objective of this research is to quantify the titanium deposition kinetics on intermediate-sized Ni wire (75 µm diameter) and determine the required coating time to achieve the desired near-equiatomic NiTi composition. It also explores an ex-situ study of the formation of a dual-pore structure that forms in some of the wires and provides insight for future in-situ investigations of the wire size effect on pack titanizing. Even though binary NiTi shape memory alloys offer excellent biocompatibility, strength, and corrosion resistance, their application is limited to less than 100 ºC. Hence, there is a need to increase the transformation temperatures for high-temperature applications, especially for aerospace applications. Certain ternary alloying additions to NiTi form high temperature shape memory alloys (HTSMAs) as there is an associated increase in the austenite-martensite transformation temperature and, therefore, have attracted considerable attention from researchers. Ni-Ti-Zr is one such HTSMA that provides the additional advantages of weight and cost reduction as compared to its platinum (Pt), gold (Au) and hafnium (Hf) counterparts. In the current research, attempts were made to produce Ni-Ti-Zr wires by co-depositing Ti and Zr on Ni wires using a halide activated pack in a single step process. The samples gained Zr content, but not enough was deposited to increase the transformation temperature. Moreover, iv a significant variation in the coating thickness was observed, resulting in a significant fluctuation in the composition. Therefore, as a first step, deposition of Zr on Ni wires was conducted to assess the feasibility of a two-step coating process to achieve the desired ternary Ni-Ti-Zr composition. The deposition kinetics, intermetallic phases formed, coating thicknesses, and composition were determined at 925 °C for various coating durations. The samples reached approximately 12-13 at. % Zr after 3 hours of coating. The as-coated wires, upon characterization via optical and laser microscopy, SEM, and EDX, displayed a core-shell structure with intermetallic phases which appeared to be Ni7Zr2 and Ni3Zr around the Ni core demonstrating the feasibility of the deposition process. The outcome of the present study will provide insight to further research regarding fabrication of these HTSMA microtubes, which can be utilized in the automotive, aerospace, and oil industries. v LIST OF FIGURES Figure 1. (a) NiTi self-expandable neurosurgical stent (b) percutaneous aortic valve realized with eNiTinol membrane [2].................................................................................... 5 Figure 2. Schematic of Shape Memory Effect: Upon cooling austenite transforms to twinned martensite, which upon applying stress deforms and forms single variant martensite. The original austenite phase is “remembered” upon heating [20]. ....... 7 Figure 3. Schematic illustration of mechanical response of pseudoelastic material [24]. ........ 9 Figure 4. Martensite start temperature as a function of Ni content (at.%) [3]. ........................ 11 Figure 5. 3D printed Nitinol rectangular block using selective laser melting [7]. .................... 12 Figure 6. Particle size distributions and resulting the austenite finish temperatures [27] ....... 13 Figure 7. Schematic representation of the particle-based ink writing process [28] ................ 14 Figure 8. Binary NiTi phase diagram. .................................................................................... 15 Figure 9. Effect of ternary alloying additions on the transformation temperatures of Nitinol SMA [14]. ...................................................................................................................... 17 Figure 10. Aluminide coating on a Ni-base material [34]. ...................................................... 19 Figure 11. Schematic showing the various constituents of the pack, the chemical reactions, and the gas-phase and solid-state diffusion. ............................................................... 20 Figure 12. Schematic of aluminum-rich coating formed on surface of a Ni wire cross-section via pack cementation. .......................................................................................... 21 Figure 13. Optical micrographs showing the growth of the coating during the aluminization process on nickel wires for (a) 300 s and (b) 600 s. The inner core is γ-Ni and the outer shell is δ-Ni2Al3 [37]. .................................................................................. 22 vi Figure 14. Effect of titanization temperature (1000 °C) on porosity within and non-uniformity of the coating [12]. .................................................................................................... 23 Figure 15. Schematic of Kirkendall experiment showing Mo wires moving inward from their original position, Kirkendall 1947 [39]. .................................................................. 25 Figure 16. Schematic of (a) direct exchange mechanism, (b) ring mechanism, and (c) vacancy mechanism of diffusion [39]. ................................................................................. 26 Figure 17. (a) Hypothetical binary A-B diffusion couple (b) SEM image of the Kirkendall voids found at the SnPb solder/Cu pad interface after aging at 1508 ºC for three days [28,42]. ................................................................................................................. 27 Figure 18. (a) Backscattered electron micrograph of a radial cross-section of a titanized Ni wire following homogenization for 4 h at 925 °C (b) EDS profile confirming the uniform near-equiatomic NiTi composition [9]. .................................................................. 28 Figure 19. Tomographic images showing the continuity of the Kirkendall pore at three different annealing times: (a) 2h (b) 4h (c) 8h (d) reconstructed cross-section, and (e) 3D visualization of a magnified section of the pore [9]. .............................................. 29 Figure 20. Arrhenius plot of intrinsic diffusivities of nickel and titanium [43]. .......................
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