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A 2024 study found that ice V and ice XIII are not simply a disordered phase and its ordered counterpart: at ambient pressure, the researchers identified a thermodynamically stable, partially ordered intermediate between them. In their experiments, this β state occupied roughly 113–120 K. The finding complicates the picture for this specific ice pair; it does not disprove hydrogen ordering in ice generally.
What the study found
Keishiro Yamashita and Thomas Loerting studied the relationship between ice V and ice XIII, a pair useful for investigating hydrogen ordering because ice XIII has a definable fully ordered configuration and its order–disorder transition is reversible at ambient pressure. They report three regimes: ice XIII is dominant below about 113 K, a partially ordered β intermediate appears from about 113 to 120 K, and ice V is dominant above about 120 K.
The authors distinguish the β state from a temporary stage on the way from one phase to another. Calorimetry showed distinct enthalpy plateaus, while the fitted ordering kinetics differed from those of ice V and ice XIII. Together with their annealing experiments, these observations led the authors to interpret β as a separate, thermodynamically stable partially ordered state—not merely a structure frozen in place before it could equilibrate.
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How hydrogen ordering differs from other changes in ice
Ice phases can differ in both the arrangement of oxygen atoms and the orientations of water molecules. Hydrogen ordering concerns the development of orientational order among water molecules; it can occur while the oxygen framework remains comparable. A partially ordered phase therefore has some orientational organization without reaching the fully ordered arrangement associated with ice XIII.
That distinction matters because a sample with limited molecular mobility can look partly ordered simply because its orientations have become kinetically trapped. Such an orientational glass is not necessarily an equilibrium phase. The study’s central claim is that, for this pair under the conditions examined, the β intermediate remains distinct when the researchers consider long annealing times and equilibrated behavior.
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How the researchers tested the phases
Yamashita and Loerting prepared ice V from ice Ih containing 0.01 M hydrochloric acid by heating it under pressure at approximately 0.5 GPa, then quenching the sample. They studied hydrogen ordering at ambient pressure using differential scanning calorimetry and isothermal annealing. The annealing approach let them compare how the material changed over time rather than relying only on a snapshot that might capture a transient state.
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Long annealing around 110–113 K could also produce better ordered ice XIII than earlier slow-cooling protocols. This highlights why time and temperature history matter: a measured degree of order may depend on whether the sample has had enough opportunity to approach equilibrium.
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What remains unknown
The study established a thermodynamic and kinetic distinction for the β intermediate, but it did not provide a detailed structural characterization of that state. Its exact molecular arrangement is therefore unresolved. The authors point to further computational work and experimental methods such as vibrational spectroscopy and neutron diffraction as ways to investigate it.
Nor does this result establish that partially ordered equilibrium intermediates occur in every ice phase or every hydrogen-ordering transition. It adds a state to the interpretation of the ice V–ice XIII system; broader conclusions require evidence from other systems.
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Why the result matters
The familiar shorthand of a hydrogen-disordered phase paired with a hydrogen-ordered counterpart can leave out intermediate behavior. This study suggests that, for ice V and ice XIII, the transition is better described with a stable partially ordered β state between the two dominant phases. The paper’s contribution is therefore a refinement of the phase picture, not a rejection of hydrogen ordering itself.
The authors note that 20 ice polymorphs were experimentally accessible, as stated in their paper’s 2024 introduction; that figure is their published count, not a verified count for 2026.
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