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Ice_V

Ice V is a high-pressure polymorph of ice, characterized by a monoclinic crystal structure with space group C2/c and 28 water molecules per unit cell, stable under moderate pressures of approximately 0.35 to 0.60 GPa and temperatures ranging from about 249 K to 273 K.^[1]^[2] It features a hydrogen-disordered network of water molecules connected by seven distinct types of hydrogen bonds, forming a complex arrangement of four- to twelve-membered rings and zigzag chains that contribute to its higher density compared to lower-pressure ices like ice II.^[1] First identified in the early 20th century through pioneering compression experiments, Ice V represents one of the intermediate-pressure phases in water's rich polymorphic landscape, exhibiting partial proton ordering and an orientational glass transition around 130 K at ambient pressure.^[3]^[1] Discovered by Bridgman in 1912 via piston-cylinder compression of water, building on earlier high-pressure studies by Tammann, Ice V's structure was later refined through X-ray diffraction studies in the 1960s, revealing its layered architecture and the role of ring threading in accommodating density increases under pressure.^[3] Unlike hexagonal ice Ih, which dominates at ambient conditions, Ice V's hydrogen disorder leads to unique thermodynamic properties, including a reversible phase transition to its fully hydrogen-ordered counterpart, ice XIII, upon cooling below 125 K at ambient pressure, often requiring acid doping to facilitate ordering. Its stability region in the water phase diagram is bounded by transitions to ice III at lower pressures, ice VI at higher pressures, and the liquid phase near 0°C, making it relevant to geophysical contexts such as the interiors of icy satellites where self-generated pressures prevail.^[2]^[4] Ice V's vibrational spectrum and partially ordered hydrogen sites have been probed through infrared and neutron scattering, highlighting its complexity and potential as a model for understanding hydrogen bonding in disordered systems.^[1] While not directly observable on Earth's surface, its study contributes to broader insights into water's anomalous behavior under compression, informing models of planetary ices and high-pressure materials science.^[4]

Structure and Properties

Crystal Structure

Ice V exhibits a monoclinic crystal structure with space group C2/c (No. 15), containing 28 water molecules per unit cell. The lattice parameters at typical formation conditions (around 0.5 GPa and 253 K) are approximately a = 9.22 Å, b = 7.54 Å, c = 10.35 Å, and β = 109.2°, with α = γ = 90°. This arrangement forms a three-dimensional framework of oxygen atoms, where each oxygen is coordinated to four others in a distorted tetrahedral geometry, connected via hydrogen bonds. The oxygen framework consists of puckered sheets of zigzag chains, reminiscent of the hexagonal sheets in ice Ih but distorted due to pressure, interconnected by additional hydrogen bonds between sheets. These sheets feature rings of 4-, 5-, 6-, and 7-membered polygons, contributing to the overall complexity of the structure.^[5] The nearest-neighbor O-O distances range from 2.76 Å to 2.87 Å, with an average of about 2.80 Å, reflecting the compressed yet flexible tetrahedral bonding under high pressure. Ice V is characterized by proton disorder in its hydrogen bonds, where the positions of hydrogen atoms are randomly distributed among possible sites.^[6] This disorder maintains the Bernal-Fowler ice rules, ensuring that each water molecule has two hydrogen atoms covalently bonded and two forming hydrogen bonds to neighboring oxygens, while the overall orientations of the dipoles are random, leading to a net zero polarization. The lattice can be visualized as layered puckered sheets stacked along the c-axis, with inter-sheet links forming a self-interpenetrating network that distinguishes Ice V from simpler ice phases.^[7]

Physical and Thermodynamic Properties

Ice V exhibits a density of approximately 1.24–1.26 g/cm³ under its stability pressures of 0.35–0.6 GPa, with the value increasing slightly as pressure rises owing to enhanced molecular packing efficiency in its monoclinic lattice. This density is notably higher than that of ambient-pressure ice Ih (0.92 g/cm³), reflecting the structural collapse of open hydrogen-bonded networks into more compact arrangements.^[8] The compressibility of Ice V is characterized by a bulk modulus of approximately 20 GPa, indicating moderate resistance to volume change under further compression, while its elastic response shows anisotropy stemming from the low-symmetry monoclinic crystal structure.^[8] Shear moduli also rise substantially compared to lower-pressure phases like ice III, contributing to overall mechanical stability in high-pressure environments.^[8] Thermodynamically, Ice V displays a thermal expansion coefficient on the order of 240 × 10⁻⁶ K⁻¹ at 0.5 GPa and near 246 K, allowing for volume adjustments with temperature while maintaining phase integrity.^[9] Its specific heat capacity at constant pressure is approximately 2.1 J/g·K around 260 K, comparable to other proton-disordered ices and reflecting vibrational contributions from hydrogen-bonded water molecules.^[10] The dielectric properties of Ice V are marked by a high static dielectric constant (ε ≈ 100), arising from the orientational disorder of molecular dipoles within the framework, which facilitates significant polarization under electric fields.^[11] This contrasts with more ordered phases and underscores the role of dynamic proton configurations in enhancing polarizability.^[12] Spectroscopic signatures provide key diagnostic tools for Ice V identification; Raman and infrared spectra reveal O-H stretching modes in the 3200–3400 cm⁻¹ range, broadened by the irregular hydrogen bonding geometry and sensitive to pressure-induced shifts.^[13] These vibrational features, along with lattice modes below 1000 cm⁻¹, distinguish Ice V from neighboring phases like ice III and VI.

Thermodynamic Stability

Formation Conditions

Ice V is thermodynamically stable within a narrow pressure-temperature regime of approximately 0.35 to 0.63 GPa and 200 to 273 K, bounded by the triple points involving Ice III at lower pressures and Ice VI at higher pressures. The lower boundary is defined by the Ice III–Ice V–liquid triple point at 0.3501 GPa and 256.164 K, while the upper boundary corresponds to the Ice V–Ice VI–liquid triple point at 0.6324 GPa and 273.31 K. In the water phase diagram, the Ice III–Ice V solid-solid boundary exhibits a positive slope of approximately 20 MPa/K, reflecting the Clapeyron relation driven by the volume and entropy differences between these phases. In contrast, the Ice V–Ice VI boundary is nearly vertical, indicating minimal temperature dependence over this pressure range. Ice V is typically synthesized in laboratory settings using piston-cylinder apparatuses or diamond anvil cells, starting from compressed liquid water or hexagonal ice (Ice Ih) as the initial material. For instance, crystallization can be achieved by cooling liquid water under constant pressure around 0.56 GPa to temperatures as low as 230 K, often monitored via in situ X-ray diffraction. Although thermodynamically unstable at ambient conditions, Ice V can persist metastably and be recovered as a polycrystalline powder when quenched below 140 K, preventing rapid transformation to lower-pressure phases like Ice Ih. The equation of state for Ice V, describing its volume as a function of pressure and temperature V(P,T), is commonly approximated using forms like the Mie-Grüneisen equation of state, which incorporates isothermal compression data. Isothermal compression relations are also fitted to the Birch-Murnaghan equation, yielding parameters such as a reference volume V₀ ≈ 8.035 × 10⁻⁴ m³/kg, bulk modulus K₀ ≈ 13.2 GPa, and its pressure derivative K₀' ≈ 6 at relevant conditions.

Phase Transitions

Ice V undergoes first-order phase transitions to adjacent high-pressure phases, characterized by discontinuities in volume and enthalpy, as well as sluggish kinetics due to the reconstructive rearrangement of hydrogen-bonded networks. The transition to Ice VI occurs above approximately 0.6 GPa over temperatures from about 200 to 273 K, featuring a volume discontinuity of ΔV ≈ -0.5 cm³/mol and an enthalpy change of ΔH ≈ 1.2 kJ/mol, reflecting the denser body-centered cubic oxygen lattice of Ice VI compared to the tetragonal structure of Ice V.^[14] At low temperatures below 110 K under pressure, Ice V transforms to the hydrogen-ordered phase Ice XIII, a recoverable monoclinic structure that requires HCl doping to facilitate proton mobility and annealing via slow cooling to enable complete ordering. This ordering transition involves a space group change from A2/a to P2₁/c, with reversible behavior observed between 100 and 120 K at pressures of 0.35–0.63 GPa, and exhibits a small volume increase alongside a 66% reduction in residual entropy.^[15] The kinetics of these transitions are notably slow owing to their reconstructive nature, which demands breaking and reforming multiple hydrogen bonds, leading to nucleation barriers estimated at 50–100 kJ/mol that hinder rapid transformation even under favorable thermodynamic conditions.^[16] Hysteresis effects are prominent in experimental observations, with supercooling and superheating up to 10 K reported in diamond anvil cell studies of Ice V boundaries, arising from the kinetic barriers that prevent equilibrium during compression or decompression cycles.^[17] The slopes of the phase boundaries involving Ice V are described by the Clapeyron equation,

\frac{dP}{dT} = \frac{\Delta H}{T \Delta V},

which quantifies the pressure-temperature dependence using measured enthalpy and volume changes; for the Ice V–Ice VI boundary, this yields a near-vertical slope consistent with the small ΔV and modest ΔH values.^[18]

History and Research

Discovery

Ice V was first synthesized and identified in 1912 by the American physicist Percy W. Bridgman during experiments on the phase behavior of water under high pressure. Using a piston-cylinder apparatus, Bridgman compressed liquid water to approximately 3,500 atm (about 0.35 GPa) at a temperature of -10°C, observing the formation of a new solid phase distinct from previously known forms.^[19] Bridgman noted this phase as occurring between Ice III and Ice VI in the pressure-temperature diagram, with preliminary density measurements indicating a value of around 1.23 g/cm³, lower than that of Ice III but higher than Ice I. These observations were made through careful monitoring of volume changes and phase boundaries during compression and cooling cycles. He designated it as the fifth solid form of water in his seminal publication.^[19] The phase was formally named Ice V in Bridgman's 1912 paper published in the Proceedings of the American Academy of Arts and Sciences, establishing the early nomenclature for high-pressure ice polymorphs.^[19] Early investigations encountered significant challenges, including the difficulty of recovering stable samples due to rapid phase transitions triggered by decompression, which often resulted in reversion to lower-pressure phases and led to initial misidentifications of the material.^[20] In the 1930s, further refinements by Bridgman and other researchers confirmed the existence of Ice V through repeated high-pressure syntheses, although achieving sample purity proved problematic owing to contamination from adjacent phases like Ice III and Ice VI during formation and handling.

Key Studies and Developments

Following the initial identification of ice V, a landmark X-ray diffraction study in 1967 by Kamb, Prakash, and Knobler determined its monoclinic crystal structure in space group C2/c, with key unit cell dimensions of a = 9.22 Å, b = 7.54 Å, c = 10.35 Å, and β = 109.2° under high-pressure conditions. Subsequent neutron diffraction in 1971 by Hamilton, Kamb, La Placa, and Prakash utilized deuterated ice samples to provide the first direct evidence of the hydrogen atom positions, revealing significant disorder consistent with the Bernal-Fowler ice rules, and laid the foundation for subsequent structural refinements.^[1] Advancements in diffraction techniques in the late 20th century enabled more precise mapping of hydrogen site probabilities through experiments on recovered ice V samples. These studies quantified the hydrogen disorder at approximately 50% occupancy across possible bond sites, highlighting the dynamic nature of proton configurations that prevent full ordering at ambient temperatures within the stability field. Computational approaches gained prominence in the 2000s, with ab initio density functional theory (DFT) simulations offering predictions of vibrational spectra and phase stability boundaries for ice V. For instance, Benoit and Marx's 2002 study reassigned hydrogen-bond centering in dense ices, including implications for ice V's proton dynamics, by modeling quantum effects on bond lengths and energies, which aligned closely with experimental infrared spectra and resolved ambiguities in earlier classical models. From 2010 to 2023, experimental techniques expanded to probe dynamic behaviors, with shock-wave compression experiments demonstrating rapid phase transitions involving ice V under extreme conditions, such as transitions to denser phases like ice VI during nanosecond-scale loading at pressures exceeding 5 GPa. Complementing this, a 2023 investigation employed machine learning-trained interatomic potentials to simulate hydrogen ordering pathways in ice V, elucidating low-energy barriers for proton rearrangements toward the ordered ice XIII phase and predicting transition kinetics at temperatures below 130 K.^[21] In 2024-2025, computational advances included deep potential-driven explorations of ice polymorph structures, confirming stability regions for ice V.^[22] Studies on ice growth rates highlighted ice V's rapid formation under pressure.^[23] Additionally, near-infrared spectroscopy probed hydrogen ordering pathways from ice V to ice XIII.^[24]

Significance and Applications

Role in Planetary Science

Higher-pressure ice phases, such as Ice VI, play significant roles in the interior models of the ice giants Uranus and Neptune, where water-rich mantles exist at pressures exceeding 1 GPa and temperatures of several hundred K.[^[25]]^[26] While Ice V itself is stable only up to approximately 0.6 GPa, metastable extensions may be relevant in certain dynamic contexts. In the case of Jupiter's moon Ganymede, Ice V is proposed to form as a high-pressure layer beneath the subsurface ocean, at pressures around 400–1200 MPa and temperatures of 250–300 K, under conditions of moderate salinity (≤10 wt% MgSO₄) and heat flux (4–44 mW m⁻²). This layer, which can reach thicknesses of up to 155 km, acts as a boundary between the saline ocean and underlying Ice VI, potentially insulating the ocean from the rocky interior and limiting water-rock interactions that could otherwise affect core dynamo processes. By enhancing the ocean's electrical conductivity and supporting induced magnetic signatures, Ice V indirectly influences Ganymede's internally generated magnetic field, as detected by the Galileo spacecraft, and may facilitate episodic "snow" formation for material transport within the ocean.^[27]^[28] For water-rich super-Earth exoplanets, interior models indicate that Ice V layers could form in the mantles of planets with substantial water fractions, affecting radial expansion, heat transport via convection, and planetary differentiation by creating barriers to material mixing between the core, ocean, and atmosphere. These layers emerge under intermediate pressure-temperature regimes, potentially stabilizing thermal profiles and influencing habitability by regulating volatile delivery to the surface.^[25] Observational evidence for such ice layers in icy bodies is indirect, derived from gravitational data collected by Voyager 2 during its 1986 flybys of Uranus and Neptune, which revealed density profiles consistent with multi-layered icy mantles, and refined by subsequent missions like Juno's gravity measurements of Jupiter's system in the 2020s that inform analogous models for icy bodies. Recent simulations incorporating phase separation in post-giant impact scenarios for Uranus highlight the role of water-rich phase segregation in explaining the planet's extreme axial tilt (~98°), matching the observed nondipolar magnetic field and low heat emission.^[29]^[26]

Experimental and Theoretical Studies

Experimental studies of Ice V primarily employ diamond anvil cells (DACs) to achieve static compression up to approximately 3 GPa, enabling the investigation of its stability and properties under controlled conditions. These experiments often integrate in-situ Raman and Brillouin scattering techniques to measure vibrational modes and elastic properties in real time, providing insights into molecular ordering and sound velocities without sample recovery. For instance, Raman spectroscopy has been used to observe phase boundaries and melting behavior of Ice V in DACs, revealing shifts in O-H stretching modes indicative of hydrogen disorder. Brillouin scattering complements this by quantifying acoustic velocities, which help derive the equation of state and anisotropic elasticity.^[30] Shock compression experiments, driven by lasers, generate transient states of Ice V at pressures ranging from 10 to 100 GPa, allowing exploration of metastable extensions beyond equilibrium conditions. These dynamic techniques probe short-lived high-pressure phases by precompressing water samples to initial states near the Ice V field before applying laser-induced shocks, which facilitate measurements of Hugoniot states and viscosity changes. Such experiments have identified Ice V signatures in release profiles and sound speed data, highlighting its role in non-equilibrium transitions relevant to rapid compression events.^[31]^[32] Theoretical approaches to Ice V rely on molecular dynamics (MD) simulations, particularly those using the TIP4P/2005 water model, to examine disorder, diffusion, and phase stability. This model accurately reproduces the proton-disordered structure of Ice V, enabling calculations of self-diffusion coefficients and radial distribution functions that capture hydrogen bond dynamics under pressure. Quantum Monte Carlo (QMC) methods provide high-accuracy ground-state energies for Ice V and related polymorphs, correcting density functional theory (DFT) approximations and confirming relative stabilities among ice phases with minimal basis set errors. These simulations have benchmarked cohesive energies, showing Ice V's intermediate density compared to Ice III and Ice VI.^[33]^[34] Recent advances from 2020 to 2025 include the development of cryogenic DACs utilizing helium as a pressure medium, which minimizes contamination and enables cleaner sample preparation for low-temperature studies of Ice V formation. Helium's inert nature and hydrostatic properties preserve sample integrity during cooling to cryogenic temperatures, facilitating precise control over phase nucleation. Additionally, AI-accelerated DFT approaches have accelerated predictions of ordered variants of Ice V, using machine-learning interatomic potentials to explore vast configuration spaces and identify low-energy structures beyond traditional methods. These tools have revealed potential proton-ordered forms stable under specific conditions, enhancing understanding of hydrogen ordering pathways.^[35]^[36] Despite these progresses, challenges persist in obtaining single-crystal data for Ice V due to its tendency to form polycrystalline aggregates during synthesis, complicating anisotropic property measurements. The rapid nucleation under pressure often results in grain boundaries that introduce defects, limiting high-resolution diffraction studies. Furthermore, entropy models for Ice V derived from pre-2010 calorimetric data require revision to account for high-temperature behavior, as recent investigations reveal intermediate states during hydrogen ordering that alter configurational contributions. Updated models incorporating these intermediates better predict phase transitions and thermal properties at elevated temperatures.^[37]^[21]

References

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https://doi.org/10.1107/S0365110X67001592
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Open questions on the structures of crystalline water ices - PMC - NIH
Aug 7, 2020 · Then the topology and ring sizes change—rather than the six-membered rings in hexagonal ice, ice V contains both smaller and larger rings. Also, ...<|control11|><|separator|>
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Apr 1, 2021 · Its monoclinic unit cell comprises 28 water molecules, which form 4-, 5-, 6-, 8-, 9-, 10-, and 12-membered rings through hydrogen bonding.3,4 ...
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Oct 31, 2008 · In this work, we investigate the hydrogen bond fluctuations in ice V and XIII with statistical mechanical techniques that use results from ...Missing: OO | Show results with:OO
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Dec 3, 2019 · Structural features Lattice parameters: a = 9.22(2) Å, b = 7.54(1) Å, c = 10.35(2) Å α = γ = 90°, β =109.2(2)° 28 molecules per unit cell.
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Elastic properties and equation of state of high pressure ice
May 15, 1986 · Both moduli increase substantially going from ice III to ice V. The bulk modulus of ice VI at 0.625 GPa is more than 50% greater than ice Ih ...
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P–V–T equations of state of ices III and V Ice III occupies the region on the P–T diagram of water substance smallest of all known stable ice polymorphs.
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At low frequencies, there was a small increase in the apparent dielectric constant E' and a ... Complex dielectric constant plots for Ice V; A, -24.2°,4200 bar; B ...
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The Raman spectra at 77°K of Ices Ih, Ic, II, III, and V made from H2O and D2O have been obtained. The spectra in the O–H and O—D stretching region were ...<|control11|><|separator|>
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Most of the high-pressure phases of ice can be recovered at ambient pressure provided that they are first cooled below about 100K. ... ice V, can be explained ...
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Jan 29, 2018 · To overcome the kinetic barriers and reach phases, which are difficult to crystallize, various doping techniques have been used. By doping ices ...
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Thermodynamics of high-pressure ice phases explored with ... - Nature
Aug 10, 2022 · Our study thus clarifies the phase behaviour of the high-pressure ices and reveals peculiar solid–solid transition mechanisms not known in other systems.
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None
Nothing is retrieved...<|control11|><|separator|>
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[PDF] notice - NASA Technical Reports Server (NTRS)
modification of the actual structure attained under pressure. Bearing in mind the well-known difficulties of recovering these high-pressure polymorphs on ...<|control11|><|separator|>
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[23]
Thermodynamically Stable Intermediate in the Course of Hydrogen ...
Jan 25, 2024 · The ice V–XIII phase transition takes place reversibly at 110–125 K and ambient pressure, (9,19) below the temperature of its irreversible ...
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Single‐Crystal Elasticity of High‐Pressure Ice up to 98 GPa by ...
Apr 6, 2021 · Here, we present direct experimental constraints on the single-crystal elasticity of ice with 0.5 mol/L (0.9 mol.%) NaCl up to 98 GPa at 300 K.
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At high pressure, it takes on a number of alternate ice forms (ice V, VI ... the Birch–Murnaghan equation of state at low pressures,. density functional ...
[26]
[PDF] Icy or Rocky? Convective or Stable? New interior models of Uranus ...
Oct 2, 2025 · We present a new framework for constructing agnostic and yet physical models for planetary interiors and apply it to Uranus and. Neptune.
[27]
[PDF] Ganymede׳s internal structure including thermodynamics of ... - HAL
Sep 30, 2024 · internally generated magnetic field in Ganymede's metallic core ... will be sandwiched between layers of ice I and ice V and VI, with the ...
[28]
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[29]
Phase separation of planetary ices explains nondipolar ... - PNAS
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Morphologies of ice crystals and their pressure-temperature melting relations were directly observed in a hydrothermal diamond-anvil cell ... ice V and ice ...
[31]
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[32]
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[33]
Efficient Determination of Water/Ice Phase Diagram through ...
Apr 20, 2025 · In this work, we report the melting points of ice Ih, III, V, and VI between 0.1 and 1190 MPa through molecular dynamics direct coexistence simulations in the ...
[34]
Fast and accurate quantum Monte Carlo for molecular crystals - PNAS
Feb 5, 2018 · DMC also predicts the correct relative energies of the ice polymorphs, yielding slightly improved lattice energies over those reported in ref.
[35]
Putting the Squeeze on Helium - National Ignition Facility
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[36]
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