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Stress Measurement and Development of Zirconium Diboride- Silicon Carbide Ceramics

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Stress Measurement and Development of Zirconium Diboride- Silicon Carbide Ceramics Scholars' Mine Doctoral Dissertations Student Theses and Dissertations Summer 2011 Stress measurement and development of zirconium diboride- silicon carbide ceramics Jeremy Lee Watts Missouri University of Science and Technology, [email protected] Follow this and additional works at: https://scholarsmine.mst.edu/doctoral_dissertations Part of the Materials Science and Engineering Commons Department: Materials Science and Engineering Recommended Citation Watts, Jeremy Lee, "Stress measurement and development of zirconium diboride-silicon carbide ceramics" (2011). Doctoral Dissertations. 2010. https://scholarsmine.mst.edu/doctoral_dissertations/2010 This thesis is brought to you by Scholars' Mine, a service of the Missouri S&T Library and Learning Resources. This work is protected by U. S. Copyright Law. Unauthorized use including reproduction for redistribution requires the permission of the copyright holder. For more information, please contact [email protected]. i STRESS MEASUREMENT AND DEVELOPMENT OF ZIRCONIUM DIBORIDE- SILICON CARBIDE CERAMICS By JEREMY LEE WATTS A DISSERTATION Presented to the Faculty of the Graduate School of the MISSOURI UNIVERSITY OF SCIENCE AND TECHNOLOGY In Partial Fulfillment of the Requirements for the Degree DOCTOR OF PHILOSOPHY in MATERIALS SCIENCE AND ENGINEERING 2011 Approved Greg Hilmas, Advisor William Fahrenholtz Richard Brow Lokesh Dharani Eric Bohannan ii iii PUBLICATION DISSERTATION OPTION Portions of this dissertation have been prepared in the style for publication in the Journal of the European Ceramic Society and the Journal of the American Ceramic Society . The manuscript entitled “Stress Measurements in ZrB 2-SiC Composites Using Raman Spectroscopy and Neutron Diffraction” was published in the Journal of the European Ceramic Society in volume 30 number 11 in 2010. The manuscript entitled “Measurement of Thermal Residual Stresses in ZrB 2-SiC Composites” was accepted for publication in the Journal of the European Ceramic Society in March 2011. The manuscript entitled “Mechanical Characterization of ZrB 2-SiC Composites with Varying SiC Particle Sizes” has been submitted to the Journal of the American Ceramic Society . The manuscript entitled “Mechanical Characterization of Annealed ZrB 2-SiC Composites” will be submitted to the Journal of the American Ceramic Society following revisions based on the dissertation committee’s suggestions. iv ABSTRACT Research presented in this dissertation focused on the production of ZrB 2- SiC composites and their characterization; in particular their mechanical properties and thermally generated residual stresses. Thermally generated stresses were measured using Raman spectroscopy as well as both neutron and x-ray diffraction. For 70 vol% ZrB 2 – 30 vol% SiC composites neutron diffraction revealed that the SiC phase was under ~880 MPa compressive stress and the ZrB 2 phase was under ~450 MPa tension at room temperature. It was also discovered that stresses began to accumulate at ~1400 °C upon cooling from the processing temperature (1900 °C -2000 °C). Raman spectroscopy and x-ray diffractions agreed well with one another and showed the stresses in the SiC phase on the surface of the samples to be ~350 MPa; lower than that in the bulk as measured by neutron diffraction. It has also been shown that annealing composites at temperatures below 1400 °C, particularly while under pressure can partially relieve these stresses leading to increases in mechanical strength of as much as 30%. The role of the particle size of the SiC phase was also investigated. For SiC particle sizes smaller than 11.5 µm, the failure strengths of the composites followed a 1/c1/2 type relationship as predicted by Griffith. Above that particle size however, strength, modulus, and hardness all decreased rapidly. It was discovered that for SiC particle sizes larger than 11.5 µm microcracking occurred resulting in the decrease of the measured mechanical properties. v AKNOWLEDGEMENTS Firstly, I would like to thank my advisor, Dr. Greg Hilmas for all his assistance and guidance throughout my graduate career. He has allowed me to travel the country as well as abroad to present my work in addition to the research opportunities he has afforded me. He has allowed me a great deal of freedom in my research without letting me wander too far off the path. I would also like to thank Dr. Fahrenholtz for providing continuous insight and support. I would also like to thank the other members of my committee, Drs. Brow, Dharani, and Bohannan. Without them, I could not be in the position that I am. Whether they are aware of it or not, each one of them have provided me with important tools or insights that have allowed me to progress in my research. I would like to acknowledge that my research was funded through the Air Force Office of Scientific Research through contract numbers FA9550-06-1-0125 and FA9550-09-1-0168 under program managers Joan Fuller, and Ali Sayir. Without their financial support this research would not have been possible. I would like to thank my friends and fellow students for all their help and support. There are too many for me to list for fear of omitting someone. I have had the great fortune to work with a great number of people whose insights have been invaluable in the progress of my research. Finally, I would like to thank my family for their unwavering support. It is because of their upbringing and guidance that I am in the position that I am today. vi TABLE OF CONTENTS Page PUBLICATION DISSERTATION OPTION........................................................... iii ABSTRACT.......................................................................................................... iv AKNOWLEDGEMENTS........................................................................................ v LIST OF FIGURES ............................................................................................... x LIST OF TABLES ............................................................................................... xv SECTION 1. INTRODUCTION.............................................................................................1 References ......................................................................................................3 2. LITERATURE REVIEW ...................................................................................4 2.1. INTRODUCTION.....................................................................................4 2.2. EARLY BORON RESEARCH..................................................................6 2.3. PROCESSING ........................................................................................8 2.3.1. Phase Equilibria of ZrB 2. ..........................................................8 2.3.2. Processing of ZrB 2. ................................................................10 2.3.3. ZrB 2-SiC Composites. ............................................................12 2.3.3.1 Hot-pressing. ............................................................12 2.3.3.2 Reactive processing. ................................................16 2.4. PROPERTIES .......................................................................................18 2.4.1. Monolithic ZrB 2.......................................................................18 2.4.2. ZrB 2 Based Composites. ........................................................22 vii 2.4.3. Particle Size Effects. ..............................................................25 2.5. RESIDUAL STRESS .............................................................................27 2.5.1. Theory....................................................................................27 2.5.2. Particulate Ceramics. .............................................................29 2.5.3. ZrB 2 Based Composites. ........................................................31 2.6. STRESS MEASUREMENTS.................................................................32 2.6.1. X-Ray Diffraction. ...................................................................32 2.6.2. Neutron Diffraction. ................................................................34 2.6.3. Raman Spectroscopy.............................................................36 2.7. ANNEALING RESIDUAL STRESS .......................................................40 References ....................................................................................................42 PAPER 1. STRESS MEASUREMENTS IN ZRB 2-SIC COMPOSITES USING RAMAN SPECTROSCOPY AND NEUTRON DIFFRACTION ....................................53 Abstract .........................................................................................................53 Introduction....................................................................................................54 Experimental Procedure ................................................................................56 Materials and Processing ..............................................................................56 Characterization ............................................................................................58 Results and Discussion .................................................................................60 Conclusions...................................................................................................67 Acknowledgements .......................................................................................67 References ....................................................................................................68
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