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«By DANIEL H. DOLAN III A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy WASHINGTON STATE ...»

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A dissertation submitted in partial fulfillment

of the requirements for the degree of

Doctor of Philosophy


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.



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.




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 compressed 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 onset 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.

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geneous nucleation at water-window interfaces.

Optical imaging measurements (0.01 mm spatial resolution, 20 ns exposures) revealed 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.

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4.1 Transmission losses in a non-absorbing sample............... 100

4.2 Measured photodiode outputs......................... 100

4.3 Photodiode transmission for experiments T1, T2, and T3.......... 103

4.4 Photodiode transmission for experiments T4................. 106

4.5 Photodiode transmission records for experiments T5 and T6......... 108

4.6 Spectrally resolved transmission for experiment T5............. 109

4.7 Photodiode transmission records for experiments T7 and T8......... 111

4.8 Loading history in quartz, sapphire, and hybrid liquid cells......... 113

4.9 Photodiode transmission records for experiments T9 and T10........ 114

4.10 Photodiode transmission records for experiments T11 and T12....... 116

4.11 Raw images from experiment I1....................... 120

4.12 Measured transmission for experiment I1................... 122

4.13 Images obtained in experiment I1....................... 123

4.14 Measured transmission for experiment I2................... 126

4.15 Images obtained in experiment I2....................... 127

4.16 Images obtained in experiment I3....................... 128

4.17 Photodiode transmission record for experiment I4.............. 130

4.18 Images obtained in experiment I4....................... 131

4.19 Raw signals of the VISAR measurement................... 134

4.20 Particle velocity history for experiment V1.................. 137

4.21 Particle velocity history for experiment V2.................. 138

4.22 VISAR measurement for experiment V3................... 140

4.23 VISAR measurements long after compression................ 141

4.24 Particle velocity history for experiment V4.................. 143

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6.1 Latent heat and growth morphology..................... 189

6.2 Volume change and wave profiles....................... 191

6.3 Extinction histories for different window configurations........... 194

6.4 Surface effects in wave profile measurements................ 196

6.5 Temperature of the water-window interface................. 199

6.6 Optical transmission in surface initiated freezing............... 203

6.7 Increasing extinction with sample thickness................. 205

6.8 Time scales and peak pressure........................ 210

6.9 Comparisons of the quartz cell photodiode experiments........... 211

6.10 Fit of the T5 photodiode record........................ 212

6.11 Incubation time and the metastable history.................. 215

6.12 Incubation time and sample thickness.................... 217

6.13 Transition time and sample thickness..................... 219

6.14 Longitudinal length scales of the freezing of water.............. 221

6.15 Consistency of the optical transmission measurements............ 223

6.16 Initiation and growth in imaging measurements............... 225

6.17 Nucleation rate and lateral freezing...................... 227

6.18 Measured transmission profile and the Rayleigh scattering limit....... 229

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D.1 Photodiode transmission for experiments G1 and G2............ 290 D.2 Transparency of shocked soda lime glass................... 291 D.3 Photodiode transmission of experiment IS1................. 294 D.4 Photodiode transmission of experiment IS2 and IS3............. 296

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F.1 Simplified view of the VISAR measurement................. 312 F.2 True versus apparent velocity in the VISAR system............. 316

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the stable phase is one that has the minimum specific Gibb’s free energy g(T, P); all other phases present under such conditions will eventually convert to the stable phase. The time required for this conversion varies greatly depending on the nature of the transition and the

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a broad interest in understanding and controlling the time scales of phase transitions in numerous system, such as atmospheric clouds [4] and biological tissues [5].

The study of phase transition dynamics requires that thermodynamic changes be made on time scales less than or equal to the transformation time. Shock waves provide a useful approach for generating rapid thermodynamic changes, and as such have been used to study polymorphic and melting transitions [6]. In contrast, shock induced freezing presents several fundamental difficulties. Shock compression in liquids leads to significant temperature increases, often producing states that are too hot for freezing. Even when freezing is thermodynamically possible, there is some time required for the transition to take place. This time may be on the order of many seconds [7], which is much longer than the typical 10−6 s duration of a shock wave experiment. Whether freezing actually occurs in shock wave loading is an issue that has not been resolved [6] and is the subject of the present study.


1.1 Objectives and approach The general objective of this work was to examine and understand shock wave induced freezing in liquid water on nanosecond time scales. Liquid water was chosen for a variety of reasons. Not only is water a material of general scientific interest [8], it has an unusually large specific heat, which reduces the temperature rise caused by shock compression. There has also been a long standing controversy regarding shock induced freezing in liquid water [6].

The specific objectives of this work were:

1. To generate P,T states such that water may freeze using shock wave techniques.

2. To perform optical and wave profile measurements in shocked water to examine and characterize changes due to freezing.

3. To construct a model that describes liquid and solid water under shock compression as well as the mixed phase state.

4. To study the nucleation mechanism (i.e. homogeneous versus heterogeneous) governing shock induced freezing.

5. To assess the characteristic time and length scales for freezing.

High pressure states were generated in liquid water using multiple shock wave compression, a method that has been applied to other liquids [9, 10]. In this technique, a thin water sample confined between two optical windows is subjected to multiple shock compression using plate impact. This process approximates isentropic compression and results in substantially lower temperatures than those in single shock compression. With this technique, water can be compressed to a state where ice VII [11] is more stable than the liquid phase.

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were also performed to examine and characterize morphological features during freezing.

Wave profiles were measured using laser interferometry [12] to obtain time-resolved mechanical changes resulting from freezing.

A mixed phase water model was constructed to simulate reverberation loading and to investigate time dependent changes caused by freezing. Complete equations of state for the liquid and solid phases were constructed using published data and thermodynamic consistency requirements [10]. Rules governing the mixed phase state and a time dependent transformation law were incorporated in the water model to examine phase transition dynamics [13–16]. The water model was incorporated into a one dimensional wave propagation code [17] for modelling the reverberation experiments.

1.2 Organization of Subsequent Chapters Chapter 2 presents a general overview of the relevant properties of liquid and solid water. A discussion of the freezing process is also given with a review of previous studies on rapid freezing in water. The specific scientific questions relevant to this work are summarized with a discussion of the overall experimental approach.

Chapter 3 describes the experimental details of the optical transmission, optical imaging, and wave profile measurements made in this work. Construction, setup, and calibration procedures are given for each type of experiment. Chapter 4 presents the results from these experiments.

Chapter 5 discusses a method for constructing the complete equation of state for a single phase. This method is used to develop models for liquid and solid water. Rules for treating a mixed phase system are postulated along with a time dependent transition rate to model the freezing process. The use of this model in a one dimensional wave propagation

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on nanosecond time scales if suitable nucleation sites are present. The relevant time and length scales of the transition are also discussed. An overall summary of this work and the resulting conclusions are given in Chapter 7.

Appendix A contains mechanical drawings for all components used in this work.

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