<i>In situ</i> high-pressure nuclear magnetic resonance crystallography in one and two dimensions

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

doi:10.1063/5.0065879

Volume 6 Issue 6

Nov. 2021

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Meier Thomas, Aslandukova Alena, Trybel Florian, Laniel Dominique, Ishii Takayuki, Khandarkhaeva Saiana, Dubrovinskaia Natalia, Dubrovinsky Leonid. In situ high-pressure nuclear magnetic resonance crystallography in one and two dimensions[J]. Matter and Radiation at Extremes, 2021, 6(6): 068402. doi: 10.1063/5.0065879

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Meier Thomas, Aslandukova Alena, Trybel Florian, Laniel Dominique, Ishii Takayuki, Khandarkhaeva Saiana, Dubrovinskaia Natalia, Dubrovinsky Leonid. In situ high-pressure nuclear magnetic resonance crystallography in one and two dimensions[J]. Matter and Radiation at Extremes, 2021, 6(6): 068402. doi: 10.1063/5.0065879

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

doi: 10.1063/5.0065879

1.
Center for High Pressure Science and Technology Advanced Research, Beijing, China
2.
Bayerisches Geoinstitut, University of Bayreuth, Bayreuth, Germany
3.
Department of Physics, Chemistry and Biology (IFM), Linköping University, SE-581 83 Linköping, Sweden
4.
Material Physics and Technology at Extreme Conditions, Laboratory of Crystallography, University of Bayreuth, Bayreuth, Germany

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Corresponding author: a)Author to whom correspondence should be addressed: thomas.meier@hpstar.ac.cn
Received Date: 2021-08-05
Accepted Date: 2021-10-04

Available Online: 2021-11-01

Publish Date: 2021-11-15

Abstract

Abstract

Recent developments in in situ nuclear magnetic resonance (NMR) spectroscopy under extreme conditions have led to the observation of a wide variety of physical phenomena that are not accessible with standard high-pressure experimental probes. However, inherent di- or quadrupolar line broadening in diamond anvil cell (DAC)-based NMR experiments often limits detailed investigation of local atomic structures, especially if different phases or local environments coexist. Here, we describe our progress in the development of high-resolution NMR experiments in DACs using one- and two-dimensional homonuclear decoupling experiments at pressures up to the megabar regime. Using this technique, spectral resolutions of the order of 1 ppm and below have been achieved, enabling high-pressure structural analysis. Several examples are presented that demonstrate the wide applicability of this method for extreme conditions research.

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References(64)

References

[1]	M. Levitt, Spin Dynamics: Basics of Nuclear Magnetic Resonance, 2nd ed., Concepts in Magnetic Resonance Part A (John Wiley & Sons, Ltd., 2009), Vol.34A, pp. 60–61.
[2]	D. M. Grant and K. H. Robin, in Encyclopedia of Magnetic Resonance, 1st ed., edited by K. H. Grant and D. M. Robin (Wiley-VCH Verlag, 2007).
[3]	N. Dubrovinskaia and L. Dubrovinsky, “Crystallography taken to the extreme,” Phys. Scr. 93, 062501 (2018).10.1088/1402-4896/aabf25
[4]	M. W. MacArthur, P. C. Driscoll, and J. M. Thornton, “NMR and crystallography—Complementary approaches to structure determination,” Trends Biotechnol. 12, 149–153 (1994).10.1016/0167-7799(94)90074-4
[5]	D. L. Bryce, “NMR crystallography: Structure and properties of materials from solid-state nuclear magnetic resonance observables,” IUCrJ 4, 350–359 (2017).10.1107/s2052252517006042
[6]	C. Martineau, “NMR crystallography: Applications to inorganic materials,” Solid State Nucl. Magn. Reson. 63–64, 1–12 (2014).10.1016/j.ssnmr.2014.07.001
[7]	H.-K. Mao, B. Chen, J. Chen, K. Li, J.-F. Lin, W. Yang, and H. Zheng, “Recent advances in high-pressure science and technology,” Matter Radiat. Extremes 1, 59–75 (2016).10.1016/j.mre.2016.01.005
[8]	T. Meier, “At its extremes: NMR at giga-pascal pressures,” in Annual Reports on NMR Spectroscopy, 93rd ed., edited by G. Webb (Elsevier, London, 2018), Chap. 1, pp. 1–74.
[9]	T. Meier, N. Wang, D. Mager, J. G. Korvink, S. Petitgirard, and L. Dubrovinsky, “Magnetic flux tailoring through Lenz lenses for ultrasmall samples: A new pathway to high-pressure nuclear magnetic resonance,” Sci. Adv. 3, eaao5242 (2017); arXiv:1706.00073.10.1126/sciadv.aao5242
[10]	T. Meier, S. Khandarkhaeva, S. Petitgirard, T. Körber, A. Lauerer, E. Rössler, and L. Dubrovinsky, “NMR at pressures up to 90 GPa,” J. Magn. Reson. 292, 44–47 (2018); arXiv:1803.05472.10.1016/j.jmr.2018.05.002
[11]	T. Meier, F. Trybel, S. Khandarkhaeva, G. Steinle-Neumann, S. Chariton, T. Fedotenko, S. Petitgirard, M. Hanfland, K. Glazyrin, N. Dubrovinskaia, and L. Dubrovinsky, “Pressure-induced hydrogen-hydrogen interaction in metallic FeH revealed by NMR,” Phys. Rev. X 9, 031008 (2019); arXiv:1902.03182.10.1103/physrevx.9.031008
[12]	T. Meier, A. P. Dwivedi, S. Khandarkhaeva, T. Fedotenko, N. Dubrovinskaia, and L. Dubrovinsky, “Table-top nuclear magnetic resonance system for high-pressure studies with in situ laser heating,” Rev. Sci. Instrum. 90, 123901 (2019); arXiv:1909.09406.10.1063/1.5128592
[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); arXiv:1803.04643.10.1016/j.pnmrs.2018.04.001
[14]	S. A. Smith, W. E. Palke, and J. T. Gerig, “The Hamiltonians of NMR. Part I,” Concepts Magn. Reson. 4, 107–144 (1992).10.1002/cmr.1820040202
[15]	G. E. Pake, “Nuclear resonance absorption in hydrated crystals: Fine structure of the proton line,” J. Chem. Phys. 16, 327–336 (1948).10.1063/1.1746878
[16]	J. W. Hennel and J. Klinowski, “Magic-angle spinning: A historical perspective,” in New Techniques in Solid-State NMR, 246th ed., Topics in Current Chemistry Vol. 2, edited by J. Klinowski (Springer, Berlin, Heidelberg, 2005), pp. 1–14.
[17]	T. Meier, T. Herzig, and J. Haase, “Moissanite anvil cell design for giga-pascal nuclear magnetic resonance,” Rev. Sci. Instrum. 85, 043903 (2014).10.1063/1.4870798
[18]	T. Meier, S. Petitgirard, S. Khandarkhaeva, and L. Dubrovinsky, “Observation of nuclear quantum effects and hydrogen bond symmetrisation in high pressure ice,” Nat. Commun. 9, 2766 (2018); arXiv:1803.07019.10.1038/s41467-018-05164-x
[19]	T. Meier, D. Laniel, M. Pena-Alvarez, F. Trybel, S. Khandarkhaeva, A. Krupp, J. Jacobs, N. Dubrovinskaia, and L. Dubrovinsky, “Nuclear spin coupling crossover in dense molecular hydrogen,” Nat. Commun. 11, 6334 (2020).10.1038/s41467-020-19927-y
[20]	M. Lee and W. I. Goldburg, “Nuclear-magnetic-resonance line narrowing by a rotating rf field,” Phys. Rev. 140, A1261–A1271 (1965).10.1103/physrev.140.a1261
[21]	T. Meier, S. Reichardt, and J. Haase, “High-sensitivity NMR beyond 200 000 atmospheres of pressure,” J. Magn. Reson. 257, 39–44 (2015).10.1016/j.jmr.2015.05.007
[22]	T. Meier, S. Khandarkhaeva, J. Jacobs, N. Dubrovinskaia, and L. Dubrovinsky, “Improving resolution of solid state NMR in dense molecular hydrogen,” Appl. Phys. Lett. 115, 131903 (2019); arXiv:1908.01150v1.10.1063/1.5123232
[23]	Y. Akahama and 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).10.1063/1.1778482
[24]	Y. Akahama and H. Kawamura, “Pressure calibration of diamond anvil Raman gauge to 310GPa,” J. Appl. Phys. 100, 043516 (2006).10.1063/1.2335683
[25]	R. R. Ernst, G. Bodenhausen, A. Wokaun, and A. G. Redfield, “Principles of nuclear magnetic resonance in one and two dimensions,” Phys. Today 42(7), 75–76 (1989).10.1063/1.2811094
[26]	E. Gregoryanz, C. Ji, P. Dalladay-Simpson, B. Li, R. T. Howie, and H.-K. Mao, “Everything you always wanted to know about metallic hydrogen but were afraid to ask,” Matter Radiat. Extremes 5, 038101 (2020).10.1063/5.0002104
[27]	R. P. Dias and I. F. Silvera, “Observation of the Wigner-Huntington transition to metallic hydrogen,” Science 355, 715–718 (2017); arXiv:1610.01634.10.1126/science.aal1579
[28]	H. Y. Geng, “Public debate on metallic hydrogen to boost high pressure research,” Matter Radiat. Extremes 2, 275–277 (2017).10.1016/j.mre.2017.10.001
[29]	D. Laniel, B. Winkler, T. Fedotenko, A. Pakhomova, S. Chariton, V. Milman, V. Prakapenka, L. Dubrovinsky, and N. Dubrovinskaia, “High-pressure polymeric nitrogen allotrope with the black phosphorus structure,” Phys. Rev. Lett. 124, 216001 (2020); arXiv:2003.02758.10.1103/physrevlett.124.216001
[30]	Y. Li, X. Feng, H. Liu, J. Hao, S. A. T. Redfern, W. Lei, D. Liu, and Y. Ma, “Route to high-energy density polymeric nitrogen t-N via He–N compounds,” Nat. Commun. 9, 722 (2018).10.1038/s41467-018-03200-4
[31]	D. Laniel, B. Winkler, E. Koemets, T. Fedotenko, M. Bykov, E. Bykova, L. Dubrovinsky, and N. Dubrovinskaia, “Synthesis of magnesium-nitrogen salts of polynitrogen anions,” Nat. Commun. 10, 4515 (2019).10.1038/s41467-019-12530-w
[32]	D. Laniel, G. Weck, and 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).10.1021/acs.inorgchem.8b01325
[33]	D. Laniel, G. Weck, G. Gaiffe, G. Garbarino, and P. Loubeyre, “High-pressure synthesized lithium pentazolate compound metastable under ambient conditions,” J. Phys. Chem. Lett. 9, 1600–1604 (2018).10.1021/acs.jpclett.8b00540
[34]	L. A. O’Dell and C. I. Ratcliffe, “Ultra-wideline 14N NMR spectroscopy as a probe of molecular dynamics,” Chem. Commun. 46, 6774–6776 (2010).10.1039/C0CC01902J
[35]	R. W. Schurko, “Ultra-wideline solid-state NMR spectroscopy,” Acc. Chem. Res. 46, 1985–1995 (2013).10.1021/ar400045t
[36]	M. Witanowski, L. Stefaniak, and G. A. Webb, “Nitrogen NMR spectroscopy,” in Annual Reports on NMR Spectroscopy, edited by G. Webb (Elsevier, 1993), Vol. 25, pp. 1–82.
[37]	R. S. Macomber and G. S. Harbison, “A complete introduction to modern NMR spectroscopy,” Phys. Today 52(1), 68 (1999).10.1063/1.882558
[38]	D. Simonova, E. Bykova, M. Bykov, T. Kawazoe, A. Simonov, N. Dubrovinskaia, and L. Dubrovinsky, “Structural study of δ-ALOOH up to 29 GPa,” Minerals 10, 1055 (2020).10.3390/min10121055
[39]	A. Sano-Furukawa, T. Hattori, K. Komatsu, H. Kagi, T. Nagai, J. J. Molaison, A. M. dos Santos, and C. A. Tulk, “Direct observation of symmetrization of hydrogen bond in δ-AlOOH under mantle conditions using neutron diffraction,” Sci. Rep. 8, 15520 (2018).10.1038/s41598-018-33598-2
[40]	S. B. Pillai, P. K. Jha, A. Padmalal, D. M. Maurya, and L. S. Chamyal, “First principles study of hydrogen bond symmetrization in δ-AlOOH,” J. Appl. Phys. 123, 115901 (2018).10.1063/1.5019586
[41]	P. Cortona, “Hydrogen bond symmetrization and elastic constants under pressure of δ-AlOOH,” J. Phys.: Condens. Matter 29, 325505 (2017).10.1088/1361-648x/aa791f
[42]	A. Sano, E. Ohtani, T. Kondo, N. Hirao, T. Sakai, N. Sata, Y. Ohishi, and T. Kikegawa, “Aluminous hydrous mineral δ-AlOOH as a carrier of hydrogen into the core-mantle boundary,” Geophys. Res. Lett. 35, L03303, https://doi.org/10.1029/2007gl031718 (2008).10.1029/2007gl031718
[43]	Y. Duan, N. Sun, S. Wang, X. Li, X. Guo, H. Ni, V. B. Prakapenka, and Z. Mao, “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).10.1016/j.epsl.2018.05.003
[44]	X. Su, C. Zhao, C. Lv, Y. Zhuang, N. Salke, L. Xu, H. Tang, H. Gou, X. Yu, Q. Sun et al., “The effect of iron on the sound velocitoes of δ-AlOOH up to 135 GPa,” Geosci. Front. 12, 937–946 (2021).10.1016/j.gsf.2020.08.012
[45]	H.-k. Mao and W. L. Mao, “Key problems of the four-dimensional Earth system,” Matter Radiat. Extremes 5, 038102 (2020).10.1063/1.5139023
[46]	A. J. Pell, G. Pintacuda, and C. P. Grey, “Paramagnetic NMR in solution and the solid state,” Prog. Nucl. Magn. Reson. Spectrosc. 111, 1–271 (2019).10.1016/j.pnmrs.2018.05.001
[47]	H. Yuan and L. Zhang, “In situ determination of crystal structure and chemistry of minerals at Earth’s deep lower mantle conditions,” Matter Radiat. Extremes 2, 117–128 (2017).10.1016/j.mre.2017.01.002
[48]	X.-J. Chen, “Exploring high-temperature superconductivity in hard matter close to structural instability,” Matter Radiat. Extremes 5, 068102 (2020).10.1063/5.0033143
[49]	N. W. Ashcroft, “Hydrogen dominant metallic alloys: High temperature superconductors?,” Phys. Rev. Lett. 92, 187002 (2004).10.1103/physrevlett.92.187002
[50]	A. P. Drozdov, M. I. Eremets, I. A. Troyan, V. Ksenofontov, and S. I. Shylin, “Conventional superconductivity at 203 kelvin at high pressures in the sulfur hydride system,” Nature 525, 73–76 (2015).10.1038/nature14964
[51]	J. Lv, Y. Sun, H. Liu, and Y. Ma, “Theory-orientated discovery of high-temperature superconductors in superhydrides stabilized under high pressure,” Matter Radiat. Extremes 5, 068101 (2020).10.1063/5.0033232
[52]	A. P. Drozdov, P. P. Kong, V. S. Minkov, S. P. Besedin, M. A. Kuzovnikov, S. Mozaffari, L. Balicas, F. F. Balakirev, D. E. Graf, V. B. Prakapenka, E. Greenberg, D. A. Knyazev, M. Tkacz, and M. I. Eremets, “Superconductivity at 250 K in lanthanum hydride under high pressures,” Nature 569, 528–531 (2019).10.1038/s41586-019-1201-8
[53]	M. Somayazulu, M. Ahart, A. K. Mishra, Z. M. Geballe, M. Baldini, Y. Meng, V. V. Struzhkin, and R. J. Hemley, “Evidence for superconductivity above 260 K in lanthanum superhydride at megabar pressures,” Phys. Rev. Lett. 122, 027001 (2019); arXiv:1808.07695.10.1103/PhysRevLett.122.027001
[54]	E. Snider, N. Dasenbrock-Gammon, R. McBride, M. Debessai, H. Vindana, K. Vencatasamy, K. V. Lawler, A. Salamat, and R. P. Dias, “Room-temperature superconductivity in a carbonaceous sulfur hydride,” Nature 586, 373–377 (2020).10.1038/s41586-020-2801-z
[55]	V. Struzhkin, B. Li, C. Ji, X.-J. Chen, V. Prakapenka, E. Greenberg, I. Troyan, A. Gavriliuk, and H.-k. Mao, “Superconductivity in La and Y hydrides: Remaining questions to experiment and theory,” Matter Radiat. Extremes 5, 028201 (2020).10.1063/1.5128736
[56]	P. P. Kong, V. S. Minkov, M. A. Kuzovnikov, S. P. Besedin, A. P. Drozdov, S. Mozaffari, et al.“Superconductivity up to 243 K in yttrium hydrides under high pressure” (unpublished) (2019).
[57]	T. Meier, F. Trybel, G. Criniti, D. Laniel, S. Khandarkhaeva, E. Koemets, T. Fedotenko, K. Glazyrin, M. Hanfland, M. Bykov, G. Steinle-Neumann, N. Dubrovinskaia, and L. Dubrovinsky, “Proton mobility in metallic copper hydride from high-pressure nuclear magnetic resonance,” Phys. Rev. B 102, 165109 (2020).10.1103/physrevb.102.165109
[58]	Y. Li, J. Hao, H. Liu, J. S. Tse, Y. Wang, and Y. Ma, “Pressure-stabilized superconductive yttrium hydrides,” Sci. Rep. 5, 9948 (2015).10.1038/srep09948
[59]	L. L. Liu, H. J. Sun, C. Z. Wang, and W. C. Lu, “High-pressure structures of yttrium hydrides,” J. Phys.: Condens. Matter 29, 325401 (2017).10.1088/1361-648X/aa787d
[60]	H.-K. Mao, B. Chen, H. Gou, K. Li, J. Liu, L. Wang, H. Xiao, and W. Yang, “2020—Transformative science in the pressure dimension,” Matter Radiat. Extremes 6, 013001 (2021).10.1063/5.0040607
[61]	C.-S. Yoo, “Chemistry under extreme conditions: Pressure evolution of chemical bonding and structure in dense solids,” Matter Radiat. Extremes 5, 018202 (2020).10.1063/1.5127897
[62]	B. Monserrat, S. E. Ashbrook, and C. J. Pickard, “Nuclear magnetic resonance spectroscopy as a dynamical structural probe of hydrogen under high pressure,” Phys. Rev. Lett. 122, 135501 (2019); arXiv:1902.10721.10.1103/PhysRevLett.122.135501
[63]	C. Ji, B. Li, W. Liu, J. S. Smith, A. Björling, A. Majumdar, W. Luo, R. Ahuja, J. Shu, J. Wang, S. Sinogeikin, Y. Meng, V. B. Prakapenka, E. Greenberg, R. Xu, X. Huang, Y. Ding, A. Soldatov, W. Yang, G. Shen, W. L. Mao, and H.-K. Mao, “Crystallography of low Z material at ultrahigh pressure: Case study on solid hydrogen,” Matter Radiat. Extremes 5, 038401 (2020).10.1063/5.0003288
[64]	D. V. Semenok, I. A. Kruglov, I. A. Savkin, A. G. Kvashnin, and A. R. Oganov, “On distribution of superconductivity in metal hydrides,” Curr. Opin. Solid State Mater. Sci 24 (2), 100808 (2020). https://doi.org/10.1016/j.cossms.2020.100808