Isobaric annealing of high-density amorphous ice between 0.3 and 1.9 GPa: in situ density values and structural changes

Salzmann, Christoph G.; Loerting, Thomas; Klotz, Stefan; Mirwald, Peter W.; Hallbrucker, Andreas; Mayer, Erwin

doi:10.1039/b510168a

Cited by 63 publications

(91 citation statements)

References 77 publications

(118 reference statements)

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“…Note in Fig. 3 that the Raman spectrum of the present HDA is quite similar to those of the previous observed HDA and VHDA at low temperatures (19,37), considering the small temperature dependence in the HDA Raman spectrum (37). The Raman spectra of HDA are substantially broader than those of crystalline ice VI and VII.…”

Section: Resultssupporting

confidence: 84%

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High density amorphous ice at room temperature

Chen

Yoo

2011

Proc. Natl. Acad. Sci. U.S.A.

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The phase diagram of water is both unusual and complex, exhibiting a wide range of polymorphs including proton-ordered or disordered forms. In addition, a variety of stable and metastable forms are observed. The richness of H 2 O phases attests the versatility of hydrogen-bonded network structures that include kinetically stable amorphous ices. Information of the amorphous solids, however, is rarely available especially for the stability field and transformation dynamics-but all reported to exist below the crystallization temperature of approximately 150-170 K below 4-5 GPa. Here, we present the evidence of high density amorphous (HDA) ice formed well above the crystallization temperature at 1 GPa-well inside the so-called "no-man's land." It is formed from metastable ice VII in the stability field of ice VI under rapid compression using dynamic-diamond anvil cell (d-DAC) and results from structural similarities between HDA and ice VII. The formation follows an interfacial growth mechanism unlike the melting process. Nevertheless, the occurrence of HDA along the extrapolated melt line of ice VII resembles the ice Ih-to-HDA transition, indicating that structural instabilities of parent ice VII and Ih drive the pressure-induced amorphization.dynamic-DAC | rapid solidication | high pressure kinetics | metastability A bundant in nature, water is a major constituent of planets and living organisms alike. The phase diagram of water exhibits a large number of polymorphs with great diversity in crystalline structure, chemical bonding, and collective interactions (1-3). The hydrogen-bond angles and topology of relatively weak hydrogen bonds (with respect to covalent OH bonds) are subject to large distortions, which, in turn, lead to proton and structural disorders and myriad phases-both stable and metastable (including amorphous). In addition to a large number (approximately 15) of known solid phases of H 2 O, there are many metastable phases. The metastable phases include both crystalline and disordered solids: high-and low-density amorphous (HDA and LDA) at low temperatures (4-11), high-and low-density water (HDW and LDW) (12), as well as crystalline phases of ice IV (13) near the melting line, VII (14) observed in the stability field of ice VI, VII′ (6,15,16) in the ice VIII stability field, and ice III in the ice II field (17). This is in addition to a whole series of intermediate structures arising from amorphorization, dipoleordering transitions, and symmetrization of hydrogen bonding (4, 5, 18). The strength of hydrogen bonds varies in these metastable structures, as does the transition dynamics that is not well understood.Recently, a very high density form of amorphous ice (VHDA) was found by isobaric annealing of HDA at 177 K and 1.9 GPa (7,19). The presence of VHDA is characterized from HDA by its high density-not by the network structure. In fact, the VHDA is a topologically isomorphic phase to HDA, arising from the different interstitial occupancy of oxygen atoms. In this regard, there could be many intermedi...

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Section: Resultssupporting

confidence: 84%

“…Experimental evidence for the presence of HDA at ambient temperature was found in both the sample's water-like, untextured morphology and in the characteristic Raman spectrum (19,37) at final pressures (or compression rates) above 1.3 GPa (or 0.1-65 GPa∕s), as shown in Fig. 3.…”

Section: Resultsmentioning

confidence: 93%

High density amorphous ice at room temperature

Chen

Yoo

2011

Proc. Natl. Acad. Sci. U.S.A.

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“…By contrast, for VHDA such a definition is not necessary, provided that the fully relaxed state has been obtained by annealing under pressure. [53] In summary we have shown that pressure-induced amorphization of cubic and hexagonal ice results in states of HDA differing slightly in structure and enthalpy, but which are similar in terms of density. Two slightly different states of HDA are produced implying that the "high-density amorphous ice" megabasin is very shallow, and probably a multitude of structures are produced at 77 K and 1 bar.…”

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confidence: 67%

High Density Amorphous Ice from Cubic Ice

et al. 2006

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Supercooled water does not behave like a simple liquid, but instead shows a number of anomalous properties.[1] These include the diffusion coefficient [2] or the kinematic viscosity [3] which show anomalous pressure dependencies on compression up to % 200 MPa, whereas beyond % 200 MPa the expected behaviour is observed. To explain these anomalies the second critical point hypothesis has been put forward, [4] in which a first-order-like phase transition between a low-(LDL) and high-density liquid (HDL) is thought to occur. LDL and HDL become indistinguishable above the second critical point, which is postulated to be in the "no man's land" around 180-220 K and 100-340 MPa, [5][6][7][8] where only crystalline ice has been observed experimentally. This model is supported by the observation that there are (at least) two different phases of amorphous water called low-(LDA) and high-density amorphous ice (HDA), [9,10] which have been found to show a first-order like transformation in compression/decompression experiments. [11,12] On heating, LDA and HDA experience a glass-transition to the highly viscous, supercooled liquids denoted low-(LDL) and high-density liquid (HDL), respectively. [13][14][15][16][17] The role of HDA in this model has become unclear since the discovery of a further distinct structural state called very-high density amorphous ice (VHDA).[18] It has lately been argued that only VHDA and LDA are homogeneous disordered structures, whereas HDA does not constitute a particular state of the HDA network.[19] This issue is still under debate, since the transition from HDA to VHDA on isothermal compression at 125 K has been found recently to be similar to the transition from LDA to HDA.[20] The detailed structures of recovered HDA and VHDA have been determined at ambient pressure and 77 K by means of neutron diffraction with isotope substitution. [21,22] These two studies contain the first experimental determination of the three site-site distribution functions (HÀH, OÀO, OÀH). For both HDA and VHDA there is no evidence in the diffraction pattern to show that it is microcrystalline rather than a genuinely amorphous structure.Herein, we show that HDA produced by pressure-induced amorphization of cubic ice (Ic) at 77 K is not the same material as "traditional" HDA produced by pressure-induced amorphization of hexagonal ice (Ih) at 77 K. [23,24] The density of both amorphous states recovered at ambient pressure is very similar; however, the X-ray structure factor as well as the phase transition characteristics in differential scanning calorimetry scans, differ in the onset temperature, enthalpy and sharpness of the exotherms.Hexagonal ice was prepared by either pipetting 0.300 mL of deionized water directly into the piston-cylinder apparatus lined with an indium container kept at 77 K, or by heating HDA close to ambient pressure to % 260 K and recovering to 77 K and 1 bar, or by Johari's procedure of decompressing HDA to 0.06 GPa and heating to 235 K.[25] Cubic ice was prepared by hyperquenching small liquid ...

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“…An alternative description of the state formed on heating would be a relaxed (denser) HDA referred to as rHDA. [38] Dilatometry and diffraction measurements reported by Winkel et al [40] indicate that when VHDA is decompressed at 140 K, it changes quasicontinuously into a relaxed or expanded form of HDA, labeled rHDA (also called eHDA). The transition sequence passes through the P-T conditions (0.4 GPa/142 K) where, as the present results suggest, relaxation and transformation of LDA occurs.…”

Section: Resultsmentioning

confidence: 99%

In situ Raman and optical microscopy of the relaxation behavior of amorphous ices under pressure

Yoshimura

Mao

Hemley

2009

J Raman Spectroscopy

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The transformation of low-density amorphous (LDA) ice produced from high-density amorphous (HDA) ice was studied up to 400 MPa as a function of temperature by in situ Raman spectroscopy and optical microscopy. Changes in these amorphous states of H 2 O were directly tracked without using emulsions to just above the crystallization temperature T x . The spectra show significant changes occurring above ∼125 K. The results are compared with data reported for the relaxation behavior of HDA, to form what we call relaxed HDA, or rHDA. We find a close connection with expanded HDA (eHDA), which is reported to exist as another metastable form in this P-T region. The observation of this temperature-induced LDA transition under pressure complements the previously observed pressure-induced reversible transition between LDA and HDA at 120-140 K. Copyright

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Isobaric annealing of high-density amorphous ice between 0.3 and 1.9 GPa: in situ density values and structural changes

Cited by 63 publications

References 77 publications

High density amorphous ice at room temperature

High density amorphous ice at room temperature

High Density Amorphous Ice from Cubic Ice

In situ Raman and optical microscopy of the relaxation behavior of amorphous ices under pressure

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