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X-Ray Scattering and Spectroscopy of Supercooled Water and Ice

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X-Ray Scattering and Spectroscopy of Supercooled Water and Ice X-ray scattering and spectroscopy of supercooled water and ice Jonas Alexander SELLBERG Doctoral Thesis in Chemical Physics Stockholm University 2014 Thesis for the Degree of Doctor of Philosophy in Chemical Physics Department of Physics AlbaNova University Center Stockholm University Stockholm, Sweden The front drawing depicts scattering of a single x-ray laser pulse hitting a droplet that contains water (lower left) or ice (upper right). Darker blue corresponds to more intense scattering. The orientation is not representative of reciprocal space. c Jonas A. Sellberg (2014) ISBN 978–91–7447–902–7 Printed by Universitetsservice US-AB, Stockholm, Sweden Paper I c Royal Society of Chemistry Publishing Paper II c Nature Publishing Group ii Strength does not come from physical capacity. It comes from an indomitable will. Mahatma Gandhi iii Abstract This thesis presents experimental studies of water and ice at near- atmospheric pressures using intense x-rays only accessible at synchrotrons and free-electron lasers. In particular, it focuses on the deeply supercooled, metastable state and its implications on ice nucleation. The local structure of the liquid phase was studied by x-ray scattering over a wide temperature range extending from 339 K down to 227 K. In order to be able to study the deeply supercooled liquid, micron-sized water droplets were evaporatively cooled in vacuum and probed by ultrashort x-ray pulses. This is to date the lowest temperature at which measurements of the structure have been performed on bulk liquid water cooled from room temperature. Upon deep supercooling, the structure evolved toward that of a low-density liquid with local tetrahedral coordination. At 230 K, where the low-density ∼ liquid structure started to dominate, the number of droplets containing ice nuclei increased rapidly. The estimated nucleation rate suggests that there is a “fragile-to-strong” transition in the dynamics of the liquid below 230 K, and its implications on water structure are discussed. Similarly, the electronic structure of deeply supercooled water was stud- ied by x-ray emission spectroscopy down to 222 K, but the spectral changes expected from the structural transformation remained absent and explana- tions are discussed. At high fluence, the non-linear dependence of the x-ray emission yield indicated that there were high valence hole densities created during the x-ray pulse length due to Auger cascades, resulting in reabsorp- tion of the x-ray emission. Finally, the hydrogen-bonded network in water was studied by x-ray ab- sorption spectroscopy and compared to various ices. It was found that the pre-edge absorption cross-section, which is associated with distorted hydro- gen bonds, could be minimized for crystalline ice grown on a hydrophobic BaF2(111) surface with low concentration of nucleation centers. v List of Publications This thesis is based on the following six papers, which will be referred to in the text by their corresponding Roman numerals. Reprints∗ were made with the permission from the publishers. I. Wide-angle X-ray diffraction and molecular dynamics study of medium-range order in ambient and hot water C. Huang, K. T. Wikfeldt, D. Nordlund, U. Bergmann, T. McQueen, J. Sellberg, L. G. M. Pettersson, A. Nilsson Physical Chemistry Chemical Physics 13, 19997-20007 (2011) II. Experimental Observation of Bulk Liquid Water Structure in ”No- man’s Land” J. A. Sellberg, C. Huang, T. A. McQueen, N. D. Loh, H. Laksmono, D. Schlesinger, R. G. Sierra, D. Nordlund, C. Y. Hampton, D. Starodub, D. P. DePonte, M. Beye, C. Chen, A. V. Martin, A. Barty, K. T. Wikfeldt, T. M. Weiss, C. Caronna, J. Feldkamp, L. B. Skinner, M. M. Seibert, M. Messerschmidt, G. J. Williams, S. Boutet, L. G. M. Pettersson, M. J. Bogan, A. Nilsson Accepted in Nature doi:10.1038/nature13266 (2014) III. Anomalous Behavior of the Homogeneous Ice Nucleation Rate in "No-man’s Land" H. Laksmono, T. A. McQueen, J. A. Sellberg, N. D. Loh, C. Huang, R. G. Sierra, D. Schlesinger, C. Y. Hampton, D. Starodub, D. P. DePonte, D. Nordlund, M. Beye, A. V. Martin, A. Barty, L. G. M. Pettersson, M. Seibert, M. Messerschmidt, G. J. Williams, S. Boutet, M. J. Bogan, A. Nilsson Manuscript ∗http://pubs.rsc.org/en/Content/ArticleLanding/2011/CP/C1CP22804H http://dx.doi.org/doi:10.1038/nature13266 vii viii List of Publications IV. Comparison of x-ray absorption spectra between water and ice: new ice data with low pre-edge absorption cross-section J. A. Sellberg, S. Kaya, V. H. Segtnan, C. Chen, T. Tyliszczak, H. Oga- sawara, D. Nordlund, L. G. M. Pettersson, A. Nilsson Submitted to Journal of Chemical Physics V. Reabsorption of Soft X-ray Emission at High X-ray Free-Electron Laser Fluences S. Schreck, M. Beye, J. A. Sellberg, T. McQueen, H. Laksmono, D. DePonte, B. Kennedy, S. Eckert, D. Schlesinger, D. Nordlund, H. Ogasawara, R. G. Sierra, V. H. Segtnan, K. Kubiceck, W. F. Schlotter, G. Dakovski, S. P. Moeller, U. Bergmann, S. Techert, L. G. M. Pettersson, Ph. Wernet, M. J. Bogan, Y. Harada, A. Nilsson, A. Föhlisch Submitted to Physical Review Letters VI. X-ray Emission Spectroscopy of Bulk Liquid Water in ”No-man’s Land” J. A. Sellberg, T. A. McQueen, H. Laksmono, S. Schreck, M. Beye, D. P. DePonte, B. O’Kennedy, D. Nordlund, R. G. Sierra, D. Schlesinger, T. Tokushima, S. Eckert, V. H. Segtnan, H. Ogasawara, K. Kubicek, S. Techert, U. Bergmann, G. L. Dakovski, W. F. Schlotter, Y. Harada, I. Zhovtobriukh, L. G. M. Pettersson, M. J. Bogan, Ph. Wernet, A. Föhlisch, A. Nilsson Manuscript The following is a list of papers to which I have contributed but that are left out in this thesis. If used in the text, they will be referred to as normal references. A. Effect of H2S on Fe Corrosion in CO2-saturated Brine E. Abelev, J. Sellberg, T. A. Ramanarayanan, S. L. Bernasek Journal of Materials Science 44, 6167-6181 (2009) B. Room Temperature Femtosecond X-ray Diffraction of Photosystem II Microcrystals J. Kern, R. Alonso-Mori, J. Hellmich, R. Tran, J. Hattne, H. Laksmono, C. Glöckner, N. Echols, R. G. Sierra, J. Sellberg, B. Lassalle-Kaiser, R. J. Gildea, P. Glatzel, R. W. Grosse-Kunstleve, M. J. Latimer, T. A. Mc- Queen, D. DiFiore, A. R. Fry, M. Messerschmidt, A. Miahnahri, D. W. Schafer, M. M. Seibert, D. Sokaras, T.-C. Weng, P. H. Zwart, W. E. White, P. D. Adams, M. J. Bogan, S. Boutet, G. J. Williams, J. Messinger, N. K. Sauter, A. Zouni, U. Bergmann, J. Yano, V. K. Yachandra Proceedings of the National Academy of Sciences 109, 9721-9726 (2012) ix C. Nanoflow electrospinning serial femtosecond crystallography R. G. Sierra, H. Laksmono, J. Kern, R. Tran, J. Hattne, R. Alonso-Mori, B. Lassalle-Kaiser, C. Glöckner, J. Hellmich, D. W. Schafer, N. Echols, R. J. Gildea, R. W. Grosse-Kunstleve, J. Sellberg, T. A. McQueen, A. R. Fry, M. Messerschmidt, A. Miahnahri, M. M. Seibert, C. Y. Hampton, D. Starodub, N. D. Loh, D. Sokaras, T.-C. Weng, P. H. Zwart, P. Glatzel, D. Milathianaki, W. E. White, P. D. Adams, G. J. Williams, S. Boutet, A. Zouni, J. Messinger, N. K. Sauter, U. Bergmann, J. Yano, V. K. Yachandra, M. J. Bogan Acta Crystallographica D68, 1584-1587 (2012) D. Energy-dispersive X-ray emission spectroscopy using an X-ray free- electron laser in a shot-by-shot mode R. Alonso-Mori, J. Kern, R. J. Gildea, D. Sokaras, T.-C. Weng, B. Lassalle- Kaiser, R. Tran, J. Hattne, H. Laksmono, J. Hellmich, C. Glöckner, N. Echols, R. G. Sierra, D. W. Schafer, J. Sellberg, C. Kenney, R. Herbst, J. Pines, P. Hart, S. Herrmann, R. W. Grosse-Kunstleve, M. J. Latimer, A. R. Fry, M. Messerschmidt, A. Miahnahri, M. M. Seibert, P. H. Zwart, W. E. White, P. D. Adams, M. J. Bogan, S. Boutet, G. J. Williams, A. Zouni, J. Messinger, P. Glatzel, N. K. Sauter, V. K. Yachandra, J. Yano, U. Bergmann Proceedings of the National Academy of Sciences 109, 19103-19107 (2012) E. Real-Time Observation of Surface Bond Breaking with an X-ray Laser M. Dell’Angela, T. Anniyev, M. Beye, R. Coffee, A. Föhlisch, J. Gladh, T. Katayama, S. Kaya, O. Krupin, A. Møgelhøj, D. Nordlund, J. K. Nørskov, H. Öberg, H. Ogasawara, H. Öström, L. G. M. Pettersson, W. F. Schlotter, J. A. Sellberg, F. Sorgenfrei, J. J. Turner, M. Wolf, W. Wurth, A. Nilsson Science 339, 1302-1305 (2013) F. Ultrafast soft x-ray emission spectroscopy of surface adsorbates using an x-ray free electron laser T. Katayama, T. Anniyev, M. Beye, R. Coffee, M. Dell’Angela, A. Föh- lisch, J. Gladh, S. Kaya, O. Krupin, A. Nilsson, D. Nordlund, W. F. Schlotter, J. A. Sellberg, F. Sorgenfrei, J. J. Turner, W. Wurth, H. Öström, H. Ogasawara Journal of Electron Spectroscopy and Related Phenomena 187, 9-14 (2013) x List of Publications G. Simultaneous Femtosecond X-ray Spectroscopy and Diffraction of Photosystem II at Room Temperature J. Kern, R. Alonso-Mori, R. Tran, J. Hattne, R. J. Gildea, N. Echols, C. Glöckner, J. Hellmich, H. Laksmono, R. G. Sierra, B. Lassalle-Kaiser, S. Koroidov, A. Lampe, G. Han, S. Gul, D. DiFiore, D. Milathianaki, A. R. Fry, A. Miahnahri, D. W. Schafer, M. Messerschmidt, M. M. Seibert, J. E. Koglin, D. Sokaras, T.-C. Weng, J. Sellberg, M. J. Latimer, R. W. Grosse-Kunstleve, P. H. Zwart, W. E. White, P. Glatzel, P. D. Adams, M. J. Bogan, G. J. Williams, S. Boutet, J. Messinger, A. Zouni, N. K. Sauter, V. K. Yachandra, U. Bergmann, J. Yano Science 340, 491-495 (2013) H. Selective Ultrafast Probing of Transient Hot Chemisorbed and Pre- cursor States of CO on Ru(0001) T.
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