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FABRICATION of TRANSPARENT CERAMIC LASER MEDIA for HIGH ENERGY LASER APPLICATIONS Karn Serivalsatit Clemson University, [email protected]

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FABRICATION of TRANSPARENT CERAMIC LASER MEDIA for HIGH ENERGY LASER APPLICATIONS Karn Serivalsatit Clemson University, Ksrvst@Yahoo.Com Clemson University TigerPrints All Dissertations Dissertations 5-2010 FABRICATION OF TRANSPARENT CERAMIC LASER MEDIA FOR HIGH ENERGY LASER APPLICATIONS Karn Serivalsatit Clemson University, [email protected] Follow this and additional works at: https://tigerprints.clemson.edu/all_dissertations Part of the Materials Science and Engineering Commons Recommended Citation Serivalsatit, Karn, "FABRICATION OF TRANSPARENT CERAMIC LASER MEDIA FOR HIGH ENERGY LASER APPLICATIONS" (2010). All Dissertations. 525. https://tigerprints.clemson.edu/all_dissertations/525 This Dissertation is brought to you for free and open access by the Dissertations at TigerPrints. It has been accepted for inclusion in All Dissertations by an authorized administrator of TigerPrints. For more information, please contact [email protected]. FABRICATION OF TRANSPARENT CERAMIC LASER MEDIA FOR HIGH ENERGY LASER APPLICATIONS A Dissertation Presented to the Graduate School of Clemson University In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy Materials Science and Engineering by Karn Serivalsatit May 2010 Accepted by: Dr. John Ballato, Committee Chair Dr. Stephen Foulger Dr. Jian Luo Dr. Eric Skaar i ABSTRACT Sesquioxides of yttrium, scandium, and lutetium, i.e., Y2O3, Sc 2O3, and Lu 2O3, have received a great deal of recent attention as potential high power solid state laser hosts. These oxides are receptive to lanthanide doping, including trivalent Er, Ho and Tm which have well known emissions at eye-safe wavelengths that can be excited using commercial diode lasers. These sesquioxides are considered superior to the more conventional yttrium aluminum garnet (YAG) due to their higher thermal conductivity, which is critical for high power laser system. Unfortunately, these oxides possess high melting temperatures, which make the growth of high purity and quality crystals using melt techniques difficult. Transparent ceramics are an attractive alternative route to laser hosts since the processing by-passes many of the challenges of refractory crystal melt growth. Moreover, transparent ceramics can possess added benefits relative to single crystals including faster production rates, the fabrication of larger sizes and composite laser structures, uniform doping concentrations, and better mechanical behavior. In order to fabricate highly transparent ceramics, the starting powders must have good dispersion and high reactivity. In this work, sesquioxide nanopowders with high sinterability were synthesized by solution precipitation techniques. For Y 2O3, the nanopowders were prepared using yttrium nitrate and ammonium hydroxide with the addition of a small amount of ammonium sulfate. Doping sulfate ions was found to reduce the agglomeration of Y 2O3 nanopowders. The Y 2O3 nanopowders with average particle size about 40 nm were obtained by calcining at 1050 °C for 4 hours. Unfortunately, this method failed to prepare well-dispersed Sc 2O3 and Lu 2O3 ii nanopowders. For Sc 2O3 and Lu 2O3, the nanopowders were synthesized by using scandium or lutetium sulfate and hexamethylenetetramine (HMT). The precipitate precursors were calcined at 1100 °C for 4 hours to yielded Sc 2O3 and Lu 2O3 nanopowders with average particle size 40 and 60 nm, respectively. Transparent sesquioxide ceramics were successfully fabricated by vacuum sintering compacts of nanopowders at high temperature. These ceramics had relatively large grain sizes, ranging from tens to hundreds of micrometers, due to significant grain growth at the final stage of sintering. These large-grained ceramics tend to not offer significant enhancements to strength or thermal shock resistance that smaller grain-sized transparent ceramics afford. Sub-micrometer-grained highly transparent sesquioxide ceramics were fabricated using a two-step sintering process followed by hot isostatic pressing (HIP). This process yielded full densification of the sesquioxide ceramics with drastically reduced grain growth. These sub-micrometer-grained ceramics exhibited a transparency equivalent to that of single crystals in the near-infrared spectral. The microhardness and fracture toughness of transparent ceramics fabricated by this method were found to exceed those of transparent ceramics fabricated by conventional sintering. The single-crystal-like transmittance of the sub-micrometer-grained yttria ceramics in the visible and IR region with high mechanical properties is an important advancement for the use of these materials in more extreme environments, including high power laser systems where reduction of scattering and thermal shock resistance are critical. iii DEDICATION This dissertation is dedicated to my parents, Vatcharin and Preeya Serivalsatit, who supported and inspired me at the every moment of my life. iv ACKNOWLEDGMENTS I would like to express my extreme gratitude to my advisor, Dr. John Ballato, for giving me the opportunity to work in his lab over the past four years. He also guided me throughout this work and provided constant support to achieve my goal. I am especially grateful for the freedom to put my own idea into this research. I wish to express my appreciation to all present and former colleagues of the Ballato research group, Baris Kokuoz, Basak Yazgan Kokuoz, Tiffany James, Andrew James, Exley McCormick, Courtney Kucera, Laura Burka, Wade Hawkins, Dr. Paul Foy, Dr. Luiz Jacobsohn, and Stephanie Morris, for their support and friendship. I would also like to acknowledge for my committee member, Dr. Jian Luo, Dr. Stephen Foulger, and Dr. Eric Skaar, for their suggestion and reviewing my dissertation. I would like to thank electron microscope facility staff, Dr. Joan Hudson, Dr. Haijun Quian, Donald Mulwee, and Dayton Cash for helping on SEM and TEM. I am particularly grateful for my parents, Vatcharin and Preeya, and my sister, Valya, who have been loving and supportive throughout my education. Most of all, I would like to thank my wife, Parinda, for her love, patience, and support. Without her support, this dissertation may have never been completed. v TABLE OF CONTENTS Page TITLE PAGE .................................................................................................................... i ABSTRACT ..................................................................................................................... ii DEDICATION ................................................................................................................ iv ACKNOWLEDGMENTS ............................................................................................... v LIST OF TABLES .......................................................................................................... ix LIST OF FIGURES ......................................................................................................... x CHAPTER I. INTRODUCTION ......................................................................................... 1 1.1 References .......................................................................................... 5 II. BACKGROUND ........................................................................................... 6 2.1 Solid state laser .................................................................................. 6 2.2 Single crystal laser medium ............................................................... 8 2.3 Transparent ceramic laser medium .................................................... 9 2.4 Fabrication of transparent ceramics ................................................. 12 2.4.1 Powder synthesis ..................................................................... 13 2.4.2 Sintering .................................................................................. 21 2.5 References ........................................................................................ 36 III. Er-DOPED Y 2O3 NANOPARTICLES: A COMPARISON OF DIFFERENT SYNTHESIS METHODS ......................................... 41 3.1 Introduction ...................................................................................... 41 3.2 Experimental procedures ................................................................. 42 3.3 Results and discussion ..................................................................... 45 3.4 Conclusions ...................................................................................... 62 3.5 References ........................................................................................ 64 vi Table of Contents (Continued) CHAPTER Page IV. SYNTHESIS, PROCESSING, AND PROPERTIES OF SUBMICROMETER-GRAINED HIGHLY TRANSPARENT YTTRIA CERAMICS ........................................................................... 66 4.1 Introduction ...................................................................................... 66 4.2 Experimental procedures ................................................................. 67 4.3 Results and discussion ..................................................................... 72 4.4 Conclusion ....................................................................................... 84 4.5 References ........................................................................................ 85 V. SUB-MICROMETER GRAIN-SIZED TRANSPARENT SCANDIA CERAMICS ........................................................................ 88 5.1 Introduction ...................................................................................... 88 5.2 Experimental procedures ................................................................
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