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Time Dependent Freezing of Water Under Multiple Shock Wave TIME DEPENDENT FREEZING OF WATER UNDER MULTIPLE SHOCK WAVE COMPRESSION By DANIEL H. DOLAN III A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy WASHINGTON STATE UNIVERSITY Department of Physics MAY 2003 °c Copyright by DANIEL H. DOLAN III, 2003 All Rights Reserved °c Copyright by DANIEL H. DOLAN III, 2003 All Rights Reserved To the Faculty of Washington State University: The members of the Committee appointed to examine the dissertation of DANIEL H. DOLAN III find it satisfactory and recommend that it be accepted. ii ACKNOWLEDGEMENTS I would like to thank my advisor, Dr. Yogendra Gupta, for suggesting, supporting, and guiding this project. I am also grateful for the assistance and insight of Dr. James John- son in developing the mixed phase water model. Many thanks go to Dr. Philip Marston for providing the water purification system and serving on the thesis committee. Dr. Matthew McCluskey and Dr. Jow-Lian Ding are also thanked for serving on the committee. The wave code calculations in this work were aided by numerous discussions with Dr. Michael Winey. I thank Dr. Oleg Fat’yanov and Dr. Scott Jones for their assis- tance in the VISAR experiments. Kurt Zimmerman played a large role in the constructing the optical imaging system and other instrumentation for this work. Dave Savage, Steve Thompson, John Rutherford, and Gary Chantler assisted in building and performing the experiments. Finally, I wish to acknowledge the support and understanding of my wife, Elizabeth. Funding for this research was provided by DOE Grant DE-FG03-97SF21388. iii TIME DEPENDENT FREEZING OF WATER UNDER MULTIPLE SHOCK WAVE COMPRESSION Abstract by Daniel H. Dolan III, Ph.D. Washington State University May 2003 Chair: Y.M. Gupta Multiple shock wave compression experiments were performed to examine the time dependence of freezing in compressed water. These experiments produced quasi-isentropic compression, generating pressures and temperatures where liquid water is metastable with respect to the ice VII phase. Time resolved optical and wave profile measurements were used in conjunction with a thermodynamically consistent equation of state and a phe- nomenological transition rate to demonstrate that water can freeze on nanosecond time scales. Single pass optical transmission measurements (ns resolution) indicated that com- pressed water loses its transparency in a time dependent manner. This change is consistent with the formation of ice regions that scatter light and reduce sample transparency. The on- set of freezing and subsequent transition were accelerated as water was compressed further past the ice VII phase boundary. Freezing was always observed when water was in contact with a silica window; the transition did not occur if only sapphire windows were present. iv These observations suggest that freezing on nanosecond time scales begins through hetero- geneous nucleation at water-window interfaces. Optical imaging measurements (0.01 mm spatial resolution, 20 ns exposures) re- vealed that freezing in compressed water is heterogeneous on 0.01-0.1 mm length scales and begins at several independent sites. As freezing progressed over time, the water sample became a complex network of opaque material separated by transparent regions of unfrozen liquid. The transition growth morphology was consistent with freezing, which is limited by the diffusion of latent heat. Laser interferometry was used to measure particle velocity histories in compressed water. The results were compared to calculated wave profiles to show that water remains a pure liquid during the initial compression stages. As compression approached a steady state, the measured particle velocity decreased when a silica window was present. This decrease suggests that the frozen material is denser than the compressed liquid. Similar particle velocity decreases were observed in the calculated wave profiles when water was allowed to remain a metastable liquid for some time. These results are consistent with the transparency loss described above, demonstrating that water can freeze on nanosecond time scales. v TABLE OF CONTENTS Page ACKNOWLEDGEMENTS iii ABSTRACT iv LIST OF TABLES xii LIST OF FIGURES xvii CHAPTER 1. Introduction . 1 1.1 Objectives and approach . 2 1.2 Organization of Subsequent Chapters . 3 References for Chapter 1 . 5 2. Background . 7 2.1 Liquid water . 7 2.1.1 Microscopic structure . 8 2.1.2 Thermodynamic and transport properties . 10 2.1.3 Optical transmission properties . 15 2.2 Solid water . 17 2.2.1 The phase diagram of water . 19 2.2.2 Solid nucleation from the liquid phase . 20 2.2.3 Freezing time scales in water . 26 2.3 Previous shock wave experiments on water . 28 2.3.1 Shock wave experiments in liquid water . 29 2.3.2 Shock induced freezing . 30 2.4 Unresolved questions and approach . 34 2.5 Multiple shock wave compression . 35 2.5.1 Multiple shock compression and plate impact . 36 2.5.2 Temperature advantages of multiple shock compression . 38 vi References for Chapter 2 . 41 3. Experimental Methods . 53 3.1 Optical transmission experiments . 53 3.1.1 Overall configuration . 53 3.1.2 Mechanical components and assembly . 55 3.1.3 Instrumentation and optical components . 61 3.1.4 Experimental setup . 63 3.2 Optical imaging experiments . 71 3.2.1 Overall configuration . 71 3.2.2 Mechanical components and assembly . 75 3.2.3 Instrumentation and optical components . 77 3.2.4 Experimental setup . 80 3.3 Wave profile experiments . 88 3.3.1 Overall configuration . 88 3.3.2 Mechanical components and assembly . 88 3.3.3 Instrumentation and optical components . 92 3.3.4 Experimental setup . 92 References for Chapter 3 . 95 4. Experimental Results . 97 4.1 Optical transmission measurements . 97 4.1.1 Determining sample transmission . 99 4.1.2 Experimental results . 102 4.1.3 Summary . 117 4.2 Optical imaging measurements . 117 4.2.1 Determining sample transmission . 119 4.2.2 Experimental results . 121 4.2.3 Summary . 129 4.3 Wave profile measurements . 132 4.3.1 Particle velocity determination . 132 4.3.2 Experimental results . 135 vii 4.3.3 Summary . 142 References for Chapter 4 . 144 5. Time Dependent Continuum Model for Water . 145 5.1 EOS development . 145 5.1.1 Thermodynamic consistency . 146 5.1.2 The form of f (T;v) for constant cv . 146 5.2 Liquid water model . 147 5.2.1 Choice of EOS . 147 5.2.2 EOS formulation . 148 5.2.3 Isentropic freezing and the value of cv . 154 5.3 Solid water model . 157 5.3.1 Assumptions . 157 5.3.2 EOS formulation . 157 5.4 Mixed phase modelling . 160 5.4.1 Mixture rules . 160 5.4.2 Time dependence of the freezing transition . 161 5.4.3 Limiting cases for isentropic compression . 162 5.5 Wave propagation calculations . 167 5.5.1 Calculation outline . 167 5.5.2 Enforcing the mixture rules . 168 5.5.3 Mixed phase calculations . 171 References for Chapter 5 . 182 6. Analysis and Discussion . 187 6.1 First order phase transition . 187 6.1.1 Latent heat . 188 6.1.2 Volume change . 188 6.2 The importance of surface effects . 190 6.2.1 Evidence for surface effects . 192 6.2.2 Surface initiated freezing . 197 6.2.3 Ice nucleation at window surfaces . 206 viii 6.3 Freezing time scales . 209 6.3.1 Apparent time scales . 209 6.3.2 Incubation time analysis . 213 6.3.3 Transition time analysis . 218 6.4 Transition length scales . 220 6.4.1 Domains of the water sample . 220 6.4.2 Lateral freezing variations . 222 6.4.3 Composition of the transformed material . 228 References for Chapter 6 . 231 7. Summary and Conclusions . 235 7.1 Summary . 235 7.2 Conclusions . 238 7.3 Recommendations for future work . 239 References for Chapter 7 . 240 APPENDIX A. Mechanical Drawings . 243 References for Appendix A . 268 B. Window Materials . 269 B.1 Soda lime glass . 269 B.2 Fused silica . 270 B.3 z-cut quartz . 271 B.4 a-cut Sapphire . 272 References for Appendix B . 273 C. Water Sample Preparation . 275 C.1 Contamination and treatment methods . 275 C.2 Sample purification . 277 C.3 Filling the liquid cell . 284 References for Appendix C . 285 ix D. Supplemental Data . ..
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