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An Ultralow-Density Porous Ice with the Largest Internal Cavity Identified in the Water Phase Diagram

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An Ultralow-Density Porous Ice with the Largest Internal Cavity Identified in the Water Phase Diagram An ultralow-density porous ice with the largest internal cavity identified in the water phase diagram Yuan Liua,b,1, Yingying Huangc,d,1, Chongqin Zhub,e,f, Hui Lia, Jijun Zhaod, Lu Wangg,2, Lars Ojamäeh, Joseph S. Franciscob,e,f,2, and Xiao Cheng Zenga,b,2 aBeijing Advanced Innovation Center for Soft Matter Science and Engineering, Beijing University of Chemical Technology, 100029 Beijing, China; bDepartment of Chemistry, University of Nebraska–Lincoln, Lincoln, NE 68588; cShanghai Advanced Research Institute, Chinese Academy of Sciences, 201210 Shanghai, China; dKey Laboratory of Materials Modification by Laser, Ion and Electron Beams, Dalian University of Technology, Ministry of Education, 116024 Dalian, China; eDepartment of Earth and Environmental Science, University of Pennsylvania, Philadelphia, PA 19104-6316; fDepartment of Chemistry, University of Pennsylvania, Philadelphia, PA 19104-6316; gCollaborative Innovation Center of Chemistry for Energy Materials, Department of Materials Science and Engineering, University of Science and Technology of China, 230026 Hefei, China; and hDepartment of Physics, Chemistry, and Biology, Linköping University, SE-58 183 Linköping, Sweden Contributed by Joseph S. Francisco, April 25, 2019 (sent for review January 15, 2019; reviewed by Ben Slater and Amadeu K. Sum) The recent back-to-back findings of low-density porous ice XVI and dictions. This porous ice phase is named ice XVI. Later, ice XVII, XVII have rekindled the century-old field of the solid-state physics a metastable porous ice phase, was also produced by emptying the and chemistry of water. Experimentally, both ice XVI and XVII crystals clathrate hydrogen hydrate (3). The mass density of both ice XVI can be produced by extracting guest atoms or molecules enclosed in and XVII is in the range of 0.81–0.85 g/cm3, lower than that the cavities of preformed ice clathrate hydrates. Herein, we examine (0.93 g/cm3) of normal ice Ih. Note that among the known more than 200 hypothetical low-density porous ices whose struc- clathrate hydrogen hydrates, the highest capacity for hydrogen tures were generated according to a database of zeolite structures. storage is 5.3 wt %, achieved by the sII type (15, 16). This record Hitherto unreported porous EMT ice, named according to zeolite hydrogen storage among ice clathrate hydrates can be broken if a nomenclature, is identified to have an extremely low density of 3 stable porous ice with a lower mass density than the sII type can be 0.5 g/cm and the largest internal cavity (7.88 Å in average radius). produced in the laboratory. Several guest-free porous ices with The EMT ice can be viewed as dumbbell-shaped motifs in a hexago- ultralow density were predicted recently via computer simulations CHEMISTRY nal close-packed structure. Our first-principles computations and mo- (9, 17, 18). One ice phase, named guest-free sIV, was predicted to lecular dynamics simulations confirm that the EMT ice is stable under be a stable phase in the temperature–pressure (T-P) phase dia- negative pressures and exhibits higher thermal stability than other ultralow-density ices. If all cavities are fully occupied by hydrogen gram of water ice at deeply negative pressures (9). molecules, the EMT ice hydrate can easily outperform the record Zeolite-like ices belong to the hypothetical low-density porous hydrogen storage capacity of 5.3 wt % achieved with sII hydro- ices because of their large cavities that can potentially be exploited gen hydrate. Most importantly, in the reconstructed temperature– for gas storage. In fact, the three most common types of ice pressure (T-P) phase diagram of water, the EMT ice is located at clathrate hydrates, sI, sII, and sH, are isostructural with various deeply negative pressure regions below ice XVI and at higher tem- silica clathrate minerals, i.e., MEP with sI, MTN with sII, and perature regions next to FAU. Last, the phonon spectra of empty-sII, DOH with sH, based on the nomenclature of zeolites (19). In FAU, EMT, and other zeolite-like ice structures are computed by particular, the tetrahedrally coordinated frameworks of oxygen in using the dispersion corrected vdW-DF2 functional. Compared with those of ice XI (0.93 g/cm3), both the bending and stretching vibra- Significance tional modes of the EMT ice are blue-shifted due to their weaker hydrogen bonds. Among 18 known ice structures, ice XVI and XVII were produced by emptying the guest atoms/molecules encapsulated in cavities porous ice | ultralow density | EMT ice | reconstructed temperature– of porous ices. We demonstrate simulation evidence that the pressure phase diagram | record hydrogen storage capacity ultralow-density porous EMT ice (named according to zeolite nomenclature) is thermodynamically stable under negative ater is a unique form of matter with many intriguing pressures. Such a low-density solid (∼60% of the mass density of Wproperties. One such physical property is its wide variety ice XVI) can be exploited for hydrogen storage with H2 mass of stable and metastable crystal structures. To date, 18 different density of 12.9 wt %, which is more than twice that (5.3 wt %) crystalline ice phases have been established experimentally (1– achieved by sII clathrate hydrate. With EMT ice, the temperature– 3). Many more ice phases ranging from 1D to 3D have been pressure phase diagram of water under negative pressures is predicted from computer simulations (4–10). Another known ice reconstructed. Like ice XVII, EMT ice could be produced by form is ice clathrate hydrates with large internal cavities that can pumping off guest molecules in EMT hydrates preformed at high host guest molecules. Clathrate natural gas hydrates have re- pressure. ceived considerable attention because they are an enormous energy source on Earth. Indeed, the amount of carbon in natural Author contributions: Y.L., L.O., J.S.F., and X.C.Z. designed research; Y.L., Y.H., L.W., and X.C.Z. performed research; C.Z., H.L., J.Z., L.O., J.S.F., and X.C.Z. contributed new reagents/ gas hydrates is estimated to be at least twice that in all other analytic tools; Y.L., Y.H., C.Z., H.L., J.Z., L.W., L.O., J.S.F., and X.C.Z. analyzed data; and Y.L., fossil energies combined (11). Clathrate hydrogen hydrates have Y.H., L.W., J.S.F., and X.C.Z. wrote the paper. also received growing attention as they are a renewable and Reviewers: B.S., University College London; and A.K.S., Colorado School of Mines. carbon-free energy source (12). The authors declare no conflict of interest. In previous computer simulation studies, guest-free clathrate Published under the PNAS license. hydrates of type sII were independently predicted to be a stable 1Y.L. and Y.H. contributed equally to this work. phase at negative pressures by Jacobson et al. (13), Conde et al. 2To whom correspondence may be addressed. Email: [email protected], frjoseph@sas. (14), and Huang et al. (8). Remarkably, the guest-free clathrate upenn.edu, or [email protected]. hydrate of type sII was recently produced in the laboratory by This article contains supporting information online at www.pnas.org/lookup/suppl/doi:10. Falenty et al. (2) by pumping off guest Ne atoms from the cav- 1073/pnas.1900739116/-/DCSupplemental. ities of sII clathrate hydrate, confirming earlier theoretical pre- www.pnas.org/cgi/doi/10.1073/pnas.1900739116 PNAS Latest Articles | 1of8 Downloaded by guest on September 28, 2021 ice can be identified to be isomorphic with the corresponding silicon frameworks in silica (17, 20–23). Hence, a large number of hypothetical zeolite-like porous ices can be generated based on the structural frameworks of zeolites in the IZA-SC database (http://www.iza-structure.org/databases/). For example, Tribello and Slater proposed hypothetical SGT and DDR clathrate hy- drates (23). Matsui et al. (17) identified ultralow-density ITT ice after examining many hypothetical zeolite-like ices. Based on first- principles computations, Liu and Ojamäe predicted a metastable crystalline ice phase, named clathrate ice sL, in the negative- pressure region (18). Engel et al. (24) predicted many crystalline ice structures from data mining of the tetrahedral zeolite net- works. Kumar et al. (25) theoretically studied how to nucleate and grow water zeolites. In this work, we examined more than 200 hypothetical low-density porous ices whose structures are generated according to a database of zeolite structures. Most importantly, we identified ultralow-density porous EMT ice that is not only energetically favorable but also thermodynamically stable in the reconstructed phase diagram of water ice. In view of its larger cavities and lower mass density than the sII type, the EMT Fig. 1. Mass densities of hypothetical zeolite-like porous ices generated from the tetrahedral frameworks of zeolite structures in the IZA-SC database ice could be a highly effective medium for gas storage. and relaxed by using the TIP4P/2005 potential in the NPT ensemble for 5 ns at 10 K and 1 bar. Results and Discussion Construction and Screening of Zeolite-Like Porous Ices. Based on the tetrahedral structural frameworks of zeolites in the IZA-SC structures, respectively. Here the larger water cavity, (H2O)60 database (http://www.iza-structure.org/databases/), more than (42166125 cage), surrounded by the dumbbell-shaped water mo- 200 hypothetical zeolite-like porous ice structures were gener- tifs is shown in Fig. 2B, and it has an average radius of 7.88 Å for 18 4 4 ated with the oxygen atoms occupying the tetrahedral positions the EMT ice. For the FAU ice, the large cavity, (H2O)48 (4 6 12 of the zeolite frameworks. For each hypothetical ice structure, cage) (SI Appendix,Fig.S1B), has an average radius of 7.16 Å.
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