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Experimental observation of liquid–solid transition of nanoconfined water at ambient temperature

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Abstract

Nanoconfined water exhibits many abnormal properties compared with bulk water. However, the origin of those anomalies remains controversial due to the lack of experimental access to the molecular-level details of the hydrogen-bonding network of water within a nanocavity. Here we address this issue by combining scanning probe microscopy with nitrogen-vacancy-centre-based quantum sensing. Such a technique allows us to characterize both dynamics and structure of water confined between a hexagonal boron nitride flake and a hydrophilic diamond surface by nanoscale nuclear magnetic resonance. We observe a liquid–solid phase transition of nanoconfined water at ambient temperature with an onset confinement size of ~1.6 nm, below which the water diffusion is considerably suppressed and the hydrogen-bonding network of water becomes structurally ordered. The complete crystallization is observed below a confinement size of ~1 nm. The liquid–solid transition is further confirmed by molecular dynamics simulation. These findings shed new light on the phase transition of nanoconfined water and may form a unified picture for understanding water anomalies at the nanoscale.

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Fig. 1: Schematics of the experimental setup and SPM measurements for the confinement size.
Fig. 2: Nanoscale NMR spectroscopy of confined water at different confinement sizes.
Fig. 3: Phase transition of nanoconfined water obtained by experiment and theoretical calculation.
Fig. 4: Structure analysis of confined water.

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Data availability

The relevant data supporting the findings of this study are available via Zenodo (https://doi.org/10.5281/zenodo.17555910)82. All other data needed to evaluate the conclusions in the paper are present in the Article or Supplementary Information. Source data are provided with this paper.

Code availability

The code used in this study for the NMR simulations is available via Zenodo (https://doi.org/10.5281/zenodo.17555910)82.

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Acknowledgements

We thank L. Yang and C. Yu from Peking University (PKU) for their help with the 2D material transfer and fabrications, and N. Zhao from Beijing Computational Science Research Center (CSRC) for meaningful guidance and discussions on the NMR simulations. This work was supported by the National Key R&D Program under grant number 2021YFA1400500; the Program under grant number 2023ZD0301300; the National Natural Science Foundation of China under grant numbers 11888101, 21725302, 12474160, U22A20260 and 12250001; the Strategic Priority Research Program of the Chinese Academy of Sciences under grant number XDB28000000; and the Beijing Municipal Science & Technology Commission under grant number Z231100006623009. W.Z. acknowledges the China Postdoctoral Science Foundation under grant number 2022M710235. Y.J. acknowledges the New Cornerstone Science Foundation through the New Cornerstone Investigator Program and the XPLORER PRIZE, and the Beijing Outstanding Young Scientist Program under grant number JWZQ20240101002. X.C.Z. acknowledges support from the Hong Kong Global STEM Professorship Scheme and the Research Grants Council of Hong Kong (GRF grant numbers 11204123 and 11302225). J.J. acknowledges funding support from the National Natural Science Foundation of China (grant number 22303072). R.S., A.D. and J.W. acknowledge the BMBF via Clusters4Future: QSens and the DFG under grant numbers FOR 2724, GRK 2642 and WR 28/34-1.

Author information

Author notes

  1. These authors contributed equally: Wentian Zheng, Shichen Zhang, Jian Jiang.

Authors and Affiliations

  1. International Center for Quantum Materials, School of Physics, Peking University, Beijing, People’s Republic of China

    Wentian Zheng, Shichen Zhang, Yipeng He, Ke Bian, En-Ge Wang & Ying Jiang

  2. Department of Material Science and Engineering, City University of Hong Kong, Hong Kong, People’s Republic of China

    Jian Jiang & Xiao Cheng Zeng

  3. Shenzhen Research Institute, City University of Hong Kong, Shenzhen, People’s Republic of China

    Jian Jiang

  4. 3rd Institute of Physics, University of Stuttgart and Institute for Quantum Science and Technology (IQST), Stuttgart, Germany

    Rainer Stöhr, Andrej Denisenko & Jörg Wrachtrup

  5. Max Planck Institute for Solid State Research, Stuttgart, Germany

    Rainer Stöhr, Andrej Denisenko & Jörg Wrachtrup

  6. Hong Kong Institute for Clean Energy, City University of Hong Kong, Hong Kong, People’s Republic of China

    Xiao Cheng Zeng

  7. Interdisciplinary Institute of Light-Element Quantum Materials and Research Center for Light-Element Advanced Materials, Peking University, Beijing, People’s Republic of China

    Ke Bian, En-Ge Wang & Ying Jiang

  8. Collaborative Innovation Center of Quantum Matter, Beijing, People’s Republic of China

    En-Ge Wang & Ying Jiang

  9. Tsientang Institute for Advanced Study, Zhejiang, People’s Republic of China

    En-Ge Wang

  10. New Cornerstone Science Laboratory, Peking University, Beijing, People’s Republic of China

    Ying Jiang

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Contributions

Y.J., K.B. and E.-G.W. supervised the project. K.B. and Y.J. designed the experiment. R.S. and A.D. grew the diamond chips and fabricated the shallow NVs. S.Z. and W.Z. transferred the hBN flakes and fabricated the hBN–diamond structure. W.Z. and S.Z. performed the experiments and data acquisition. W.Z., S.Z., J.J., K.B., Y.H., J.W., X.C.Z., Y.J. and E.-G.W. performed the experimental data analysis and interpretation. J.J. and X.C.Z. performed the MD simulations. W.Z., S.Z., J.J. and K.B. performed the NMR simulations. W.Z., K.B., S.Z., J.J., X.C.Z., Y.J. and E.-G.W. wrote the manuscript with input from all other authors. All authors commented on the final manuscript.

Corresponding authors

Correspondence to Xiao Cheng Zeng, Ke Bian, En-Ge Wang or Ying Jiang.

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Nature Materials thanks Giancarlo Franzese, Francesco Paesani and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Extended data

Extended Data Fig. 1 Determine the thickness of the intrinsic water layer on the diamond surface.

(a) Topographic image of diamond surface without the hBN flake, corresponding to the open system. The position of the NV center was determined by the procedures described in Supplementary Fig. 1, denoted as an orange dashed circle with the nearby reference protrusion being marked by an arrow. (b) Topographic image of the same area with the hBN flake and without confined water molecules, which was confirmed by the nanoscale-NMR measurement. (c) Z-profile was measured along the dashed line in (a) (black) and in (b) (red). The position of the NV center was estimated with an uncertainty denoted by the shades. The measured height difference of the two profiles indicates the thickness of the intrinsic water layer on the diamond surface: dwater = 2.7 ± 0.2 nm. Scale bar: 250 nm.

Source data

Extended Data Fig. 2 Nanoscale-NMR spectroscopies showing beating features under the strong confinement measured by two different NVs.

(a) Left panel: correlation spectroscopy at a confinement size of 0.7 ± 0.3 nm measured by an NV with depth of 4.39 ± 0.49 nm. By using a sum of cosine functions with multiple frequencies and an exponentially decayed envelope \(S\left(\widetilde{\tau }\right)={e}^{-\widetilde{\tau }/{T}_{{\rm{corr}}}}{\sum }_{i}{S}_{i}\cos \left({2\pi f}_{i}\widetilde{{\rm{\tau }}}+{\varphi }_{i}\right)\), the signal was fitted with a time constant of Tcorr = 183.7 ± 29.5 µs. Right panel: the corresponding power spectrum showing a multi-peak feature. (b) Left panel: correlation spectroscopy at a confinement size of 1.5 ± 0.4 nm measured by an NV with depth of 5.13 ± 0.65 nm. The signal was fitted with a time constant of Tcorr = 224.3 ± 45.1 µs. Right panel: the corresponding power spectrum showing two peaks.

Source data

Extended Data Fig. 3 Influence of surface functionalization on the diffusivity of nanoconfined water.

(a) The hydroxylated (100) surface with carbonyl(-C = O), ether(C-O-C), and hydroxyl(-OH) functional groups, and (b) the methoxy-acetone oxidized diamond (100) surface with carbonyl(-C = O) and ether(C-O-C) functional groups adopted for classical MD simulation. Red, white, and gray balls represent oxygen, hydrogen, and carbon atoms, respectively. (c) The calculated diffusion coefficients of the whole water layer in three different confinement systems from MD simulation: (1) Water confined between a hydroxylated hydrophilic diamond surface and a hydrophobic hBN surface (gray), (2) water confined between a methoxy-acetone oxidized hydrophilic diamond surface and a hydrophobic hBN surface (red), and (3) water confined between two hydrophobic hBN surfaces (blue). Dt are presented as mean values ± standard deviations, derived from 3 simulations.

Source data

Extended Data Fig. 4 MD simulation of the rotational coefficients of the whole water layer.

Rotational coefficients (Dr) were calculated through the statistical trajectories of water molecules, for dconfine ranging from 1 nm to 6 nm, where they exhibited a large suppression at dconfine < 2 nm. Dr are presented as mean values ± standard deviations, derived from 3 simulations.

Source data

Extended Data Fig. 5 Calculation of the bond-order parameter.

Calculated local q6 Steinhardt parameters of the confined water layer with dconfine ranging from 0.6 nm to 6 nm by using the TIP4P/Ice model. q6 bond-order parameter quantifies the six-fold symmetry of the hydrogen bond structures. The results show increased ordering with decreasing confinement size, with two transition points of slope change (marked by arrows) at approximately 2.1 nm and 1.2 nm, respectively. The increase in q6 at ~2.1 nm indicates the onset of the liquid-solid transition, while the sharp increase in q6 at ~1.2 nm indicates the rapid crystallization.

Source data

Supplementary information

Supplementary Information

Supplementary Texts 1–8, Table 1, Figs. 1–11 and refs. 1–21.

Supplementary Data 1

Raw data for Supplementary Fig. 1.

Supplementary Data 2

Raw data for Supplementary Fig. 2c,d.

Supplementary Data 3

Raw data for Supplementary Fig. 3b.

Supplementary Data 4

Raw data for Supplementary Fig. 4b.

Supplementary Data 5

Raw data for Supplementary Fig. 5.

Supplementary Data 6

Raw data for Supplementary Fig. 8.

Supplementary Data 7

Raw data for Supplementary Fig. 10d,e.

Supplementary Data 8

Raw data for Supplementary Fig. 11.

Source data

Source Data Fig. 1

Raw data for Figs. 1d–g.

Source Data Fig. 2

Raw data for Fig. 2a–c.

Source Data Fig. 3

Raw data for Fig. 3a,b.

Source Data Fig. 4

Raw data and code for Fig. 4d.

Source Data Extended Data Fig. 1

Raw data for Extended Data Fig. 1a–c.

Source Data Extended Data Fig. 2

Raw data for Extended Data Fig. 2.

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Raw data for Extended Data Fig. 3.

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Raw data for Extended Data Fig. 4.

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Raw data for Extended Data Fig. 5.

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Zheng, W., Zhang, S., Jiang, J. et al. Experimental observation of liquid–solid transition of nanoconfined water at ambient temperature. Nat. Mater. (2026). https://doi.org/10.1038/s41563-025-02456-8

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