Recrystallisation of HDA ice under pressure by in-situ neutron diffraction to 3.9 GPa

  • S. Klotz
  • , G. Hamel
  • , J. S. Loveday
  • , R. J. Nelmes
  • , M. Guthrie

Research output: Contribution to journalReview articlepeer-review

67 Scopus citations

Abstract

We have studied by in-situ neutron diffraction the recrystallisation behaviour of HDA ice in the pressure range 0.3-3.9 GPa, i.e. the entire stability range of HDA. We report quantitative and detailed structural information on the various high pressure ice phases formed metastably at low temperatures. We find that between ∼0.4-0.7 GPa, HDA transforms at 175 K to mainly phases IV and V, and XII, and at 1-1.2 GPa to a mixture of ice VI and XII. On isothermal compression at 100 K, HDA recrystallises to an ice VII-like structure which is either partially ordered or mixed with ice VIII. Full structural data obtained by Rietveld refinements are reported for all these phases at low temperatures. Phases IV, V and XII are fully hydrogen disordered when obtained from HDA. The transformation behaviour in the 0.5-1.2 GPa range is in good agreement with the picture reported from quenched-recovered samples, although some differences persist in the recrystallisation to IV/XII mixtures. The recrystallisation behaviour of HDA over the entire pressure range appears to follow closely that of liquid water under pressure.

Original languageEnglish
Pages (from-to)117-122
Number of pages6
JournalZeitschrift fur Kristallographie
Volume218
Issue number2
DOIs
StatePublished - 2003
Externally publishedYes

Funding

results and conclusions with D. D. Klug, M. Saitta, M. C. Bellissent-Funel, and A. Hallbrucker. We thank D. J. Francis and J. Dreyer for help in the experiments. Our work (JSL, RJN, MG) is funded by a research grant from EPSRC, and supported by CCLRC through access to beamtime and other resources.

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