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The observation of square ice in graphene questioned

Nature volume 528, pages E1–E2 (2015)Cite this article

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A Brief Communications Arising to this article was published on 23 December 2015

A Brief Communications Arising to this article was published on 23 December 2015

ARISING FROM G. Algara-Siller et al. Nature 519, 443–445 (2015); doi:10.1038/nature14295

Algara-Siller et al.1 reported the observation of a new phase of water—‘square ice’—sandwiched between two graphene layers at room temperature. Their key evidence consists of transmission electron microscope (TEM) images of a square lattice from small encapsulated crystals, the detection of oxygen from relatively large regions containing such crystals and molecular dynamics (MD) simulations indicating ‘square ice’ formation inside hydrophobic nanochannels. Here we propose that the reported experimental data can be better explained by salt (for example, NaCl) contaminants precipitating as nanocrystals in the dried-out graphene liquid cells2 and common oxide contaminants in graphene. Consequently, we question the observation of room-temperature ‘square ice’. There is a Reply to this Brief Communication Arising by Algara-Siller, G. et al. Nature 528, http://dx.doi.org/10.1038/nature16149 (2015) relating to the electron energy-loss spectra (EELS) and a Reply by Wang, F. C. et al. Nature 528, http://dx.doi.org/10.1038/nature16146 (2015) relating to the MD simulations.

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Figure 1: Structure and analysis of NaCl nanoplatelets and reported ‘square ice’.

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Authors and Affiliations

  1. Materials Science & Technology Division, Oak Ridge National Laboratory, Oak Ridge, 37831, Tennessee, USA

    Wu Zhou, Kuibo Yin, Yuyang Zhang, Albina Borisevich, Matthew F. Chisholm, Sokrates T. Pantelides & Andrew R. Lupini

  2. SEU-FEI Nano-Pico Center, Key Lab of MEMS of Ministry of Education, Southeast University, Nanjing, 210096, China

    Kuibo Yin, Tao Xu & Litao Sun

  3. Department of Physics, University of Illinois at Chicago, Chicago, 60607, Illinois, USA

    Canhui Wang & Robert F. Klie

  4. Department of Physics and Astronomy, Vanderbilt University, Nashville, 37235, Tennessee, USA

    Yuyang Zhang & Sokrates T. Pantelides

  5. Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, 37831, Tennessee, USA

    Juan Carlos Idrobo

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  1. Wu Zhou
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  2. Kuibo Yin
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  7. Litao Sun
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  11. Robert F. Klie
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Contributions

W.Z., C.W. and A.R.L. wrote this Comment with help from the other authors. W.Z., K.Y., C.W. and T.X. performed the experiment. Y.Z. and S.T.P. performed the calculations. C.W., T.X. and L.S. prepared the graphene samples. All authors discussed the paper and contributed to data analysis.

Corresponding author

Correspondence to Wu Zhou.

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Declared none.

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Zhou, W., Yin, K., Wang, C. et al. The observation of square ice in graphene questioned. Nature 528, E1–E2 (2015). https://doi.org/10.1038/nature16145

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