Venture into Water's No Man's Land: Structural Transformations of Solid ${\mathbf{H}}_{\mathbf{2}}\mathrm{O}$ under Rapid Compression and Decompression

Venture into Water’s No Man’s Land: Structural Transformations of Solid $H_{2} O$ under Rapid Compression and Decompression

Chuanlong Lin, Jesse S. Smith, Xuqiang Liu, John S. Tse, and Wenge Yang

Phys. Rev. Lett. 121, 225703 – Published 30 November 2018

Abstract

Pressure-induced formation of amorphous ices and the low-density amorphous (LDA) to high-density amorphous (HDA) transition have been believed to occur kinetically below a crossover temperature ( $T_{c}$ ) above which thermodynamically driven crystalline-crystalline (e.g., ice $I_{h}$ -to-II) transitions and crystallization of HDA and LDA are dominant. Here we show compression-rate-dependent formation of a high-density noncrystalline (HDN) phase transformed from ice $I_{c}$ above $T_{c}$ , bypassing crystalline-crystalline transitions under rapid compression. Rapid decompression above $T_{c}$ transforms HDN to a low-density noncrystalline (LDN) phase which crystallizes spontaneously into ice $I_{c}$ , whereas slow decompression of HDN leads to direct crystallization. The results indicate the formation of HDA and the HDN-to-LDN transition above $T_{c}$ are results of competition between (de)compression rate, energy barrier, and temperature. The crossover temperature is shown to have an exponential relationship with the threshold compression rate. The present results provide important insight into the dynamic property of the phase transitions in addition to the static study.

Received 11 June 2018

DOI:https://doi.org/10.1103/PhysRevLett.121.225703

Physics Subject Headings (PhySH)

Pressure effects Structural phase transition Transition temperature

Ice Molecular solids

Compaction Liquid nitrogen cooling X-ray powder diffraction

Condensed Matter, Materials & Applied Physics

Authors & Affiliations

Chuanlong Lin¹, Jesse S. Smith², Xuqiang Liu^1,3, John S. Tse^1,4,*, and Wenge Yang^1,†

¹Center for High Pressure Science and Technology Advanced Research, Shanghai 201203, China
²HPCAT, Geophysical Laboratory, Carnegie Institution of Washington, Argonne, Illinois 60439, USA
³Key Laboratory for Anisotropy and Texture of Materials, School of Material Science and Engineering, Northeastern University, Shenyang 110819, China
⁴Department of Physics and Engineering Physics, University of Saskatchewan, Saskatoon, S7N 5E2 Canada

^*Corresponding author. john.tse@usask.ca
^†Corresponding author. yangwg@hpstar.ac.cn

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Vol. 121, Iss. 22 — 30 November 2018

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Figure 1
Compression-rate-dependent formation of the high-density noncrystalline phase. (a) Under slow compression ( $< 0.01 GPa / s$ ) from $\sim 1 Pa$ to 5 GPa at an interval of $\sim 0.05 GPa$ with the pressure monitored by an on-line ruby system, the phase transition sequence of $ice I_{c} \to ice II \to ice VI \to ice VIII$ is observed. The diffraction data is acquired with exposure time of 5 s. (b) Under rapid compression from $\sim 1 Pa$ to 3.5 GPa with a rate of $\sim 14.8 GPa / s$ , ice $I_{c}$ transforms to a noncrystalline phase first, followed by crystallization into ice VIII. During rapid compression, the pressure is increased continuously with the continuous collection of x-ray diffraction images. It should be noted that the rate changes during compression process. The rate of $\sim 14.8 GPa / s$ is estimated in the pressure range where ice $I_{c}$ to HDN transition occurs. The exposure time for each diffraction image is 50 ms with images collected at a frequency of 20 Hz. (c) Summary of compression-rate-dependent phase transformation from ice $I_{c}$ to high-density noncrystalline phase at different temperatures. (d) Comparison of the diffraction patterns of the noncrystalline phases at different temperatures. The high-density noncrystalline phases above 145 K are obtained from ice $I_{c}$ under rapid compression. The HDA phases below 145 K are obtained by static compression of ice $I_{h}$ [20].
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Figure 2
Crystallization of high-density noncrystalline phase at 1.2 and 2.1 GPa by warming. (a) HDN is heated from 150 to 177 K. It starts to crystallize into ice XII at $\sim 169 K$ , and completes at $\sim 177 K$ . (b) HDN is heated from 150 K. It crystallizes into ice VI at $\sim 170 K$ and is complete at $\sim 176 K$ . (c),(d) Azimuthally unwrapped x-ray diffraction images of ice XII and VI crystallized from HDN at $\sim 1.2$ and $\sim 2.1 GPa$ , respectively. The diffraction images, subtracted by an image of the noncrystalline phase as background, are obtained by caking (unrolling) the two-dimensional x-ray diffraction images. The horizontal axis is $Q$ value. The vertical axis is azimuth angle. The white broad band at $\sim 2.3 Å^{- 1}$ indicates the first sharp peak of HDN. The black dots are the diffraction peaks from crystalline phases of ice XII and VI. The half ellipses are the masks from the area detector.
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Figure 3
Rate-dependent phase transformation of HDN at 158 K under decompression. (a) Slow decompression of HDN leads to crystallization into ice VI, followed by $ice VI \to ice II \to ice I_{c}$ transitions. (b) Rapid decompression ( $\sim 10 GPa / s$ ) of HDN results in the direct transformation to a low-density noncrystalline phase.
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Figure 4
(De)compression-rate-dependent (negative decompression, positive compression) formation of noncrystalline phases at different temperatures. Black solid triangles represent high-density noncrystalline phase obtained by rapid compression in present work. Open squares and circles indicate the high-density amorphous and low-density phases previously obtained by static compression or decompression [20]. Open triangles are low-density noncrystalline phase formed from high-pressure ice VIII under rapid decompression [33]. Red dashed line is the fitting line.
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Physical Review Letters

Venture into Water’s No Man’s Land: Structural Transformations of Solid H2O under Rapid Compression and Decompression

Chuanlong Lin, Jesse S. Smith, Xuqiang Liu, John S. Tse, and Wenge Yang

Phys. Rev. Lett. 121, 225703 – Published 30 November 2018

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Venture into Water’s No Man’s Land: Structural Transformations of Solid $H_{2} O$ under Rapid Compression and Decompression