Synthesis of Hydrothermal Degradation Resistant Nano Yttria Stabilized Zirconia

Submitted in partial fulfilment of the requirements of the degree of Master of Technology

By

Hrishikesh Rajiv Jugade

10311015

Supervisor:

Prof. Parag Bhargava

Department of Metallurgical Engineering and Materials Science INDIAN INSTITUTE OF TECHNOLOGY BOMBAY (2012)

Abstract
Yttria Stabilized Zirconia (YSZ) is an important ceramic material for dental and other biomedical applications on account of its high strength and fracture toughness due to presence of metastable tetragonal phase. Synthesis of nanocrystalline YSZ has also become important due to improvement in sinterability of nano powders. YSZ, however, suffers from a major drawback in that it undergoes tetragonal to monoclinic phase transformation in presence of moisture at relatively low temperatures. This is known as hydrothermal degradation or low temperature degradation of YSZ. Review of literature shows that resistance to degradation depends on grain size, stabilizer amount and stabilizer type. However, mechanism by which this transformation takes place is not very clear. To study the hydrothermal degradation in YSZ, 1.5 (mol %) and 3 (mol%) YSZ powders (tetragonal) were prepared by co-precipitation method and sintered at 1200C. The sintered samples of density greater than 99% and grain size less than 300 nm were subjected to hydrothermal degradation at 150C for 40 hrs in presence of water. A number of such experiments were carried out keeping the same conditions of temperature and time. The samples were then characterized using techniques such as XRD, Raman spectroscopy, FESEM etc. It was found that 1.5YSZ underwent hydrothermal degradation forming around 29% of monoclinic phase. The yttrium concentration within individual grains was found to be inhomogeneous indicating segregation of yttrium at grain boundaries. Hardness of 1.5YSZ samples decreased after hydrothermal degradation experiment. On the other hand 3YSZ samples showed extremely high resistance to hydrothermal degradation under given conditions without transforming into monoclinic phase. Their hardness remained unchanged. It was confirmed using XRD and Raman spectra that tetragonal was the only phase present in 3YSZ samples. Zirconia samples doped with 1.5 mol% of both tantalum oxide and yttrium oxide were also synthesized, sintered and studied for hydrothermal degradation. They were found to be easily susceptible to tetragonal to monoclinic phase transformation.

Acknowledgment
I sincerely thank my supervisor, Prof Parag Bhargava, for offering me the opportunity to work on this project and guiding me throughout the year. I am grateful to Mr S B Patil, Ms Preeti Bajpai Mr Shyama, PhD students of the Powder Metallurgy lab of IIT Bombay, for sharing the basics of zirconia synthesis and helping me whenever I needed. Their suggestions and guidance have been very valuable. I would like to express my gratitude towards the students and staff of various analytical research facilities of IIT Bombay, including and especially Mr Pramod, Mr Sandipan, Mr Hitesh, Mr Shekhar, Mr Sudipto, Mr Akshay Ms Vinita, Mrs Neelam, Mr Venkat, Mr Dhoke and Mrs Charlotte. I am also thankful to the people of Powder Metallurgy lab, students and staff, including Debabrata, Venumadhav, Pawan, Apoorv, Nitin, Johns, Lekha, Pragyensh and all others who were ready to help me whenever I needed.