In situ high-pressure nuclear magnetic resonance crystallography in one and two dimensions

Thomas Meier; Alena Aslandukova; Florian Trybel; Dominique Laniel; Takayuki Ishii; Saiana Khandarkhaeva; Natalia Dubrovinskaia; Leonid Dubrovinsky

doi:10.1063/5.0065879

[1] M.Levitt. Spin Dynamics: Basics of Nuclear Magnetic Resonance, 60-61(2009).

[2] D. M.Grant, K. H.Grant, K. H.Robin, H.Grant K., D. M.Robin. Encyclopedia of Magnetic Resonance(2007).

[3] L.Dubrovinsky, N.Dubrovinskaia. Crystallography taken to the extreme. Phys. Scr., 93, 062501(2018).

[4] J. M.Thornton, P. C.Driscoll, M. W.MacArthur. NMR and crystallography—Complementary approaches to structure determination. Trends Biotechnol., 12, 149-153(1994).

[5] D. L.Bryce. NMR crystallography: Structure and properties of materials from solid-state nuclear magnetic resonance observables. IUCrJ, 4, 350-359(2017).

[6] C.Martineau. NMR crystallography: Applications to inorganic materials. Solid State Nucl. Magn. Reson., 63–64, 1-12(2014).

[7] H.-K.Mao, J.Chen, H.Zheng, J.-F.Lin, K.Li, B.Chen, W.Yang. Recent advances in high-pressure science and technology. Matter Radiat. Extremes, 1, 59-75(2016).

[8] G.Webb, T.Meier. At its extremes: NMR at giga-pascal pressures. Annual Reports on NMR Spectroscopy, 1-74(2018).

[9] T.Meier, J. G.Korvink, D.Mager, S.Petitgirard, L.Dubrovinsky, N.Wang. Magnetic flux tailoring through Lenz lenses for ultrasmall samples: A new pathway to high-pressure nuclear magnetic resonance. Sci. Adv., 3, eaao5242(2017).

[10] T.Meier, S.Khandarkhaeva, S.Petitgirard, A.Lauerer, E.R?ssler, L.Dubrovinsky, T.K?rber. NMR at pressures up to 90 GPa. J. Magn. Reson., 292, 44-47(2018).

[11] S.Khandarkhaeva, K.Glazyrin, G.Steinle-Neumann, N.Dubrovinskaia, M.Hanfland, T.Fedotenko, F.Trybel, T.Meier, S.Petitgirard, S.Chariton, L.Dubrovinsky. Pressure-induced hydrogen-hydrogen interaction in metallic FeH revealed by NMR. Phys. Rev. X, 9, 031008(2019).

[12] N.Dubrovinskaia, A. P.Dwivedi, T.Fedotenko, L.Dubrovinsky, S.Khandarkhaeva, T.Meier. Table-top nuclear magnetic resonance system for high-pressure studies with in situ laser heating. Rev. Sci. Instrum., 90, 123901(2019).

[13] T.Meier. Journey to the centre of the Earth: Jules Vernes’ dream in the laboratory from an NMR perspective. Prog. Nucl. Magn. Reson. Spectrosc., 106–107, 26-36(2018).

[14] W. E.Palke, S. A.Smith, J. T.Gerig. The Hamiltonians of NMR. Part I. Concepts Magn. Reson., 4, 107-144(1992).

[15] G. E.Pake. Nuclear resonance absorption in hydrated crystals: Fine structure of the proton line. J. Chem. Phys., 16, 327-336(1948).

[16] J.Klinowski, J. W.Hennel, J.Klinowski. Magic-angle spinning: A historical perspective. New Techniques in Solid-State NMR, 1-14(2005).

[17] J.Haase, T.Herzig, T.Meier. Moissanite anvil cell design for giga-pascal nuclear magnetic resonance. Rev. Sci. Instrum., 85, 043903(2014).

[18] S.Khandarkhaeva, T.Meier, S.Petitgirard, L.Dubrovinsky. Observation of nuclear quantum effects and hydrogen bond symmetrisation in high pressure ice. Nat. Commun., 9, 2766(2018).

[19] T.Meier, D.Laniel, L.Dubrovinsky, N.Dubrovinskaia, J.Jacobs, M.Pena-Alvarez, A.Krupp, S.Khandarkhaeva, F.Trybel. Nuclear spin coupling crossover in dense molecular hydrogen. Nat. Commun., 11, 6334(2020).

[20] W. I.Goldburg, M.Lee. Nuclear-magnetic-resonance line narrowing by a rotating rf field. Phys. Rev., 140, A1261-A1271(1965).

[21] J.Haase, T.Meier, S.Reichardt. High-sensitivity NMR beyond 200 000 atmospheres of pressure. J. Magn. Reson., 257, 39-44(2015).

[22] N.Dubrovinskaia, L.Dubrovinsky, J.Jacobs, T.Meier, S.Khandarkhaeva. Improving resolution of solid state NMR in dense molecular hydrogen. Appl. Phys. Lett., 115, 131903(2019).

[23] Y.Akahama, H.Kawamura. High-pressure Raman spectroscopy of diamond anvils to 250 GPa: Method for pressure determination in the multimegabar pressure range. J. Appl. Phys., 96, 3748(2004).

[24] H.Kawamura, Y.Akahama. Pressure calibration of diamond anvil Raman gauge to 310GPa. J. Appl. Phys., 100, 043516(2006).

[25] A.Wokaun, G.Bodenhausen, A. G.Redfield, R. R.Ernst. Principles of nuclear magnetic resonance in one and two dimensions. Phys. Today, 42, 75-76(1989).

[26] H.-K.Mao, B.Li, P.Dalladay-Simpson, C.Ji, R. T.Howie, E.Gregoryanz. Everything you always wanted to know about metallic hydrogen but were afraid to ask. Matter Radiat. Extremes, 5, 038101(2020).

[27] R. P.Dias, I. F.Silvera. Observation of the Wigner-Huntington transition to metallic hydrogen. Science, 355, 715-718(2017).

[28] H. Y.Geng. Public debate on metallic hydrogen to boost high pressure research. Matter Radiat. Extremes, 2, 275-277(2017).

[29] T.Fedotenko, N.Dubrovinskaia, V.Prakapenka, L.Dubrovinsky, S.Chariton, V.Milman, D.Laniel, B.Winkler, A.Pakhomova. High-pressure polymeric nitrogen allotrope with the black phosphorus structure. Phys. Rev. Lett., 124, 216001(2020).

[30] H.Liu, X.Feng, Y.Ma, Y.Li, W.Lei, D.Liu, J.Hao, S. A. T.Redfern. Route to high-energy density polymeric nitrogen t-N via He–N compounds. Nat. Commun., 9, 722(2018).

[31] B.Winkler, E.Koemets, M.Bykov, E.Bykova, N.Dubrovinskaia, T.Fedotenko, D.Laniel, L.Dubrovinsky. Synthesis of magnesium-nitrogen salts of polynitrogen anions. Nat. Commun., 10, 4515(2019).

[32] G.Weck, D.Laniel, P.Loubeyre. Direct reaction of nitrogen and lithium up to 75 GPa: Synthesis of the Li₃N, LiN, LiN₂, and LiN₅ compounds. Inorg. Chem., 57, 10685-10693(2018).

[33] G.Garbarino, G.Gaiffe, G.Weck, D.Laniel, P.Loubeyre. High-pressure synthesized lithium pentazolate compound metastable under ambient conditions. J. Phys. Chem. Lett., 9, 1600-1604(2018).

[34] C. I.Ratcliffe, L. A.O’Dell. Ultra-wideline ¹⁴N NMR spectroscopy as a probe of molecular dynamics. Chem. Commun., 46, 6774-6776(2010).

[35] R. W.Schurko. Ultra-wideline solid-state NMR spectroscopy. Acc. Chem. Res., 46, 1985-1995(2013).

[36] M.Witanowski, L.Stefaniak, G.Webb, G. A.Webb. Nitrogen NMR spectroscopy. Annual Reports on NMR Spectroscopy, 1-82(1993).

[37] G. S.Harbison, R. S.Macomber. A complete introduction to modern NMR spectroscopy. Phys. Today, 52, 68(1999).

[38] D.Simonova, N.Dubrovinskaia, A.Simonov, L.Dubrovinsky, E.Bykova, T.Kawazoe, M.Bykov. Structural study of δ-ALOOH up to 29 GPa. Minerals, 10, 1055(2020).

[39] J. J.Molaison, A.Sano-Furukawa, T.Nagai, A. M.dos Santos, K.Komatsu, C. A.Tulk, H.Kagi, T.Hattori. Direct observation of symmetrization of hydrogen bond in δ-AlOOH under mantle conditions using neutron diffraction. Sci. Rep., 8, 15520(2018).

[40] D. M.Maurya, P. K.Jha, S. B.Pillai, A.Padmalal, L. S.Chamyal. First principles study of hydrogen bond symmetrization in δ-AlOOH. J. Appl. Phys., 123, 115901(2018).

[41] P.Cortona. Hydrogen bond symmetrization and elastic constants under pressure of δ-AlOOH. J. Phys.: Condens. Matter, 29, 325505(2017).

[42] N.Hirao, T.Kikegawa, Y.Ohishi, T.Sakai, N.Sata, T.Kondo, E.Ohtani, A.Sano. Aluminous hydrous mineral δ-AlOOH as a carrier of hydrogen into the core-mantle boundary. Geophys. Res. Lett., 35, L03303(2008).

[43] S.Wang, X.Li, Z.Mao, X.Guo, N.Sun, H.Ni, Y.Duan, V. B.Prakapenka. Phase stability and thermal equation of state of δ-AlOOH: Implication for water transportation to the deep lower mantle. Earth Planet. Sci. Lett., 494, 92-98(2018).

[44] H.Gou, X.Yu, H.Tang, L.Xu, C.Lv, X.Su, Y.Zhuang, N.Salke, Q.Sun, C.Zhao et al. The effect of iron on the sound velocitoes of δ-AlOOH up to 135 GPa. Geosci. Front., 12, 937-946(2021).

[45] H.-k.Mao, W. L.Mao. Key problems of the four-dimensional Earth system. Matter Radiat. Extremes, 5, 038102(2020).

[46] C. P.Grey, A. J.Pell, G.Pintacuda. Paramagnetic NMR in solution and the solid state. Prog. Nucl. Magn. Reson. Spectrosc., 111, 1-271(2019).

[47] L.Zhang, H.Yuan. In situ determination of crystal structure and chemistry of minerals at Earth’s deep lower mantle conditions. Matter Radiat. Extremes, 2, 117-128(2017).

[48] X.-J.Chen. Exploring high-temperature superconductivity in hard matter close to structural instability. Matter Radiat. Extremes, 5, 068102(2020).

[49] N. W.Ashcroft. Hydrogen dominant metallic alloys: High temperature superconductors?. Phys. Rev. Lett., 92, 187002(2004).

[50] A. P.Drozdov, M. I.Eremets, V.Ksenofontov, I. A.Troyan, S. I.Shylin. Conventional superconductivity at 203 kelvin at high pressures in the sulfur hydride system. Nature, 525, 73-76(2015).

[51] Y.Ma, J.Lv, Y.Sun, H.Liu. Theory-orientated discovery of high-temperature superconductors in superhydrides stabilized under high pressure. Matter Radiat. Extremes, 5, 068101(2020).

[52] M.Tkacz, S. P.Besedin, D. E.Graf, F. F.Balakirev, E.Greenberg, V. S.Minkov, M. I.Eremets, M. A.Kuzovnikov, L.Balicas, D. A.Knyazev, A. P.Drozdov, S.Mozaffari, V. B.Prakapenka, P. P.Kong. Superconductivity at 250 K in lanthanum hydride under high pressures. Nature, 569, 528-531(2019).

[53] Z. M.Geballe, M.Ahart, A. K.Mishra, Y.Meng, R. J.Hemley, M.Baldini, V. V.Struzhkin, M.Somayazulu. Evidence for superconductivity above 260 K in lanthanum superhydride at megabar pressures. Phys. Rev. Lett., 122, 027001(2019).

[54] E.Snider, A.Salamat, R.McBride, H.Vindana, K.Vencatasamy, R. P.Dias, K. V.Lawler, N.Dasenbrock-Gammon, M.Debessai. Room-temperature superconductivity in a carbonaceous sulfur hydride. Nature, 586, 373-377(2020).

[55] E.Greenberg, V.Prakapenka, X.-J.Chen, H.-k.Mao, B.Li, A.Gavriliuk, C.Ji, V.Struzhkin, I.Troyan. Superconductivity in La and Y hydrides: Remaining questions to experiment and theory. Matter Radiat. Extremes, 5, 028201(2020).

[56] P. P.Kong, S. P.Besedin, V. S.Minkov, S.Mozaffari, A. P.Drozdov, M. A.Kuzovnikov et al. Superconductivity up to 243 K in yttrium hydrides under high pressure(2019).

[57] N.Dubrovinskaia, M.Hanfland, K.Glazyrin, T.Fedotenko, L.Dubrovinsky, D.Laniel, M.Bykov, T.Meier, F.Trybel, G.Criniti, E.Koemets, S.Khandarkhaeva, G.Steinle-Neumann. Proton mobility in metallic copper hydride from high-pressure nuclear magnetic resonance. Phys. Rev. B, 102, 165109(2020).

[58] H.Liu, Y.Li, J.Hao, Y.Ma, Y.Wang, J. S.Tse. Pressure-stabilized superconductive yttrium hydrides. Sci. Rep., 5, 9948(2015).

[59] C. Z.Wang, L. L.Liu, H. J.Sun, W. C.Lu. High-pressure structures of yttrium hydrides. J. Phys.: Condens. Matter, 29, 325401(2017).

[60] W.Yang, H.Xiao, H.-K.Mao, J.Liu, H.Gou, K.Li, B.Chen, L.Wang. 2020—Transformative science in the pressure dimension. Matter Radiat. Extremes, 6, 013001(2021).

[61] C.-S.Yoo. Chemistry under extreme conditions: Pressure evolution of chemical bonding and structure in dense solids. Matter Radiat. Extremes, 5, 018202(2020).

[62] B.Monserrat, C. J.Pickard, S. E.Ashbrook. Nuclear magnetic resonance spectroscopy as a dynamical structural probe of hydrogen under high pressure. Phys. Rev. Lett., 122, 135501(2019).

[63] E.Greenberg, X.Huang, A.Soldatov, W.Yang, R.Xu, S.Sinogeikin, Y.Meng, A.Majumdar, W.Liu, G.Shen, B.Li, C.Ji, J. S.Smith, A.Bj?rling, V. B.Prakapenka, J.Shu, H.-K.Mao, W. L.Mao, Y.Ding, W.Luo, J.Wang, R.Ahuja. Crystallography of low Z material at ultrahigh pressure: Case study on solid hydrogen. Matter Radiat. Extremes, 5, 038401(2020).

[64] D. V.Semenok, I. A.Savkin, I. A.Kruglov, A. R.Oganov, A. G.Kvashnin. On distribution of superconductivity in metal hydrides. Curr. Opin. Solid State Mater. Sci(2020).