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5. Fast anion reorientations in ammine yttrium borohydride compounds Y(BH4)3·xNH3 (x = 3 and 7): a nuclear magnetic resonance study.

Author

Babanova, O. A., Skoryunov, R. V., Soloninin, A. V., and Skripov, A. V.

Abstract

Metal borohydrides are the ionic compounds which have attracted significant recent attention due to their potential applications as materials for hydrogen storage and solid electrolytes. The ammine borohydride compounds Y(BH4)3·xNH3 belong to the emerging class of materials, where the application-relevant properties can be tuned by introducing neutral NH3 ligands. To study the dynamical properties of Y(BH4)3·3NH3 and Y(BH4)3·7NH3, we have measured the 1H and 11B nuclear spin–lattice relaxation rates and nuclear magnetic resonance (NMR) spectra in these compounds over a wide temperature range (6–298 K). Our measurements have revealed that both compounds retain the unusually high reorientational mobility of BH4− anions down to low temperatures. In particular, for the fastest BH4 reorientational process, the corresponding H jump rate is of the order of 108 s−1 near 96 K in Y(BH4)3·3NH3 and near 33 K in Y(BH4)3·7NH3. The fast reorientational motion of BH4− anions is discussed in terms of the coordination environment of BH4 groups in Y(BH4)3·xNH3. [ABSTRACT FROM AUTHOR]

Published
2024
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11. Anion reorientations and the phase transition in nido-KB11H14: 1H and 11B NMR studies.

Author

Babanova, O. A., Skoryunov, R. V., Soloninin, A. V., and Skripov, A. V.

Abstract

The potassium nido-hydroborate KB11H14 exhibits high K-ion conductivity above the order–disorder phase transition temperature, ~ 400 K. To study the dynamical properties of this compound at the microscopic level, we have measured the 1H and 11B nuclear magnetic resonance spectra and spin–lattice relaxation rates over the temperature range of 148–418 K. Our measurements have revealed the fast reorientational motion of the large cluster-like nido-[B11H14]− anions. In the ordered triclinic low-T phase, this reorientational motion is characterized by the activation energy of 0.53(2) eV, and the corresponding reorientational jump rate reaches ~ 108 s−1 at 393 K. It has been found that the transition from the ordered triclinic phase to the disordered cubic phase with high ionic conductivity is accompanied by the dramatic two-orders-of-magnitude acceleration of the anion reorientations. This result supports the idea that the anion reorientational motion in alkali-metal hydroborates facilitates the cation diffusive mobility. The activation energy for the anion reorientations in the disordered high-T phase of KB11H14 is estimated to be 0.19(3) eV. [ABSTRACT FROM AUTHOR]

Published
2022
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12. Nuclear magnetic resonance study of hydrogen dynamics in the complex hydride LiBH4 · NH3.

Author

Skoryunov, R. V., Babanova, O. A., Soloninin, A. V., Grinderslev, J., Skripov, A. V., and Jensen, T. R.

Subjects
NUCLEAR magnetic resonance, PROTON magnetic resonance, SPIN-lattice relaxation, JUMP processes, HYDROGEN
Abstract

To study the dynamical properties of the complex hydride LiBH4 · NH3 we have measured proton nuclear magnetic resonance spectra and spin-lattice relaxation rates for this compound in a wide temperature range (18 – 287 K). Our measurements have revealed several jump processes with different characteristic rates. It has been shown that the spin-lattice relaxation rates in the entire studied temperature range are governed by reorientations of BH4 groups. The experimental data suggest a coexistence of at least four types of BH4 reorientations. The parameters of reorientational motion in LiBH4 · NH3 have been evaluated using the standard four-peak model. [ABSTRACT FROM AUTHOR]

Published
2022
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14. Promoting Persistent Superionic Conductivity in Sodium Monocarba-closo-dodecaborate NaCB11H12 via Confinement within Nanoporous Silica

Author

Andersson, Mikael S., primary, Stavila, Vitalie, additional, Skripov, Alexander V., additional, Dimitrievska, Mirjana, additional, Psurek, Malgorzata T., additional, Leão, Juscelino B., additional, Babanova, Olga A., additional, Skoryunov, Roman V., additional, Soloninin, Alexei V., additional, Karlsson, Maths, additional, and Udovic, Terrence J., additional

Published
2021
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15. Promoting Persistent Superionic Conductivity in Sodium Monocarba-closo-dodecaborate NaCB11H12 via Confinement within Nanoporous Silica

Author

Andersson, Mikael, Stavila, Vitalie, Skripov, Alexander, V, Dimitrievska, Mirjana, Psurek, Malgorzata T., Leao, Juscelino B., Babanova, Olga A., Skoryunov, Roman, V, Soloninin, Alexei, V, Karlsson, Maths, Udovic, Terrence J., Andersson, Mikael, Stavila, Vitalie, Skripov, Alexander, V, Dimitrievska, Mirjana, Psurek, Malgorzata T., Leao, Juscelino B., Babanova, Olga A., Skoryunov, Roman, V, Soloninin, Alexei, V, Karlsson, Maths, and Udovic, Terrence J.

Abstract

Superionic phases of bulk anhydrous salts based on large cluster-like polyhedral (carba)borate anions are generally stable only well above room temperature, rendering them unsuitable as solid-state electrolytes in energy-storage devices that typically operate at close to room temperature. To unlock their technological potential, strategies are needed to stabilize these superionic properties down to subambient temperatures. One such strategy involves altering the bulk properties by confinement within nanoporous insulators. In the current study, the unique structural and ion dynamical properties of an exemplary salt, NaCB11H12, nanodispersed within porous, high-surface-area silica via salt-solution infiltration were studied by differential scanning calorimetry, X-ray powder diffraction, neutron vibrational spectroscopy, nuclear magnetic resonance, quasielastic neutron scattering, and impedance spectroscopy. Combined results hint at the formation of a nanoconfined phase that is reminiscent of the high-temperature superionic phase of bulk NaCB11H12, with dynamically disordered CB11H12-anions exhibiting liquid-like reorientational mobilities. However, in contrast to this high-temperature bulk phase, the nanoconfined NaCB11H12 phase with rotationally fluid anions persists down to cryogenic temperatures. Moreover, the high anion mobilities promoted fast-cation diffusion, yielding Na+ superionic conductivities of similar to 0.3 mS/cm at room temperature, with higher values likely attainable via future optimization. It is expected that this successful strategy for conductivity enhancement could be applied as well to other related polyhedral (carba)borate-based salts. Thus, these results present a new route to effectively utilize these types of superionic salts as solid-state electrolytes in future battery applications.

Published
2021
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21. Anion reorientations and cation diffusion in a carbon-substituted sodium nido-borate Na-7,9-C2B9H12: 1H and 23Na NMR studies.

Author

Skripov, Alexander V., Babanova, Olga A., Skoryunov, Roman V., Soloninin, Alexei V., and Udovic, Terrence J.

Subjects
IONIC conductivity, SPIN-lattice relaxation, PHASE transitions, NUCLEAR magnetic resonance, ANIONS, SOLID electrolytes, SUPERIONIC conductors
Abstract

Polyhydroborate-based salts of lithium and sodium have attracted much recent interest as promising solid-state electrolytes for energy-related applications. A member of this family, sodium dicarba-nido-undecahydroborate Na-7,9-C2B9H12 exhibits superionic conductivity above its order-disorder phase transition temperature, ∼360 K. To investigate the dynamics of the anions and cations in this compound at the microscopic level, we have measured the 1H and 23Na nuclear magnetic resonance (NMR) spectra and spin-lattice relaxation rates over the temperature range of 148–384 K. It has been found that the transition from the low-T ordered to the high-T disordered phase is accompanied by an abrupt, several-orders-of-magnitude acceleration of both the reorientational jump rate of the complex anions and the diffusive jump rate of Na+ cations. These results support the idea that reorientations of large [C2B9H12]− anions can facilitate cation diffusion and, thus, the ionic conductivity. The apparent activation energies for anion reorientations obtained from the 1H spin-lattice relaxation data are 314 meV for the ordered phase and 272 meV for the disordered phase. The activation energies for Na+ diffusive jumps derived from the 23Na spin-lattice relaxation data are 350 and 268 meV for the ordered and disordered phases, respectively. [ABSTRACT FROM AUTHOR]

Published
2022
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26. Anion reorientations and cation diffusion in a carbon-substituted sodium nido-borate Na-7,9-C2B9H12: 1H and 23Na NMR studies

Author

Skripov, Alexander V., Babanova, Olga A., Skoryunov, Roman V., Soloninin, Alexei V., and Udovic, Terrence J.

Abstract

Polyhydroborate-based salts of lithium and sodium have attracted much recent interest as promising solid-state electrolytes for energy-related applications. A member of this family, sodium dicarba-nido-undecahydroborate Na-7,9-C2B9H12exhibits superionic conductivity above its order-disorder phase transition temperature, ∼360 K. To investigate the dynamics of the anions and cations in this compound at the microscopic level, we have measured the 1H and 23Na nuclear magnetic resonance (NMR) spectra and spin-lattice relaxation rates over the temperature range of 148–384 K. It has been found that the transition from the low-Tordered to the high-Tdisordered phase is accompanied by an abrupt, several-orders-of-magnitude acceleration of both the reorientational jump rate of the complex anions and the diffusive jump rate of Na+cations. These results support the idea that reorientations of large [C2B9H12]−anions can facilitate cation diffusion and, thus, the ionic conductivity. The apparent activation energies for anion reorientations obtained from the 1H spin-lattice relaxation data are 314 meV for the ordered phase and 272 meV for the disordered phase. The activation energies for Na+diffusive jumps derived from the 23Na spin-lattice relaxation data are 350 and 268 meV for the ordered and disordered phases, respectively.

Published
2022
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27. Low-Temperature Rotational Tunneling of Tetrahydroborate Anions in Lithium Benzimidazolate-Borohydride Li2(bIm)BH4

Author

Skripov, Alexander V., primary, Dimitrievska, Mirjana, additional, Babanova, Olga A., additional, Skoryunov, Roman V., additional, Soloninin, Alexei V., additional, Morelle, Fabrice, additional, Filinchuk, Yaroslav, additional, Faraone, Antonio, additional, Wu, Hui, additional, Zhou, Wei, additional, and Udovic, Terrence J., additional

Published
2019
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28. Promoting Persistent Superionic Conductivity in Sodium Monocarba-closo-dodecaborate NaCB11H12via Confinement within Nanoporous Silica

Author

Andersson, Mikael S., Stavila, Vitalie, Skripov, Alexander V., Dimitrievska, Mirjana, Psurek, Malgorzata T., Leão, Juscelino B., Babanova, Olga A., Skoryunov, Roman V., Soloninin, Alexei V., Karlsson, Maths, and Udovic, Terrence J.

Abstract

Superionic phases of bulk anhydrous salts based on large cluster-like polyhedral (carba)borate anions are generally stable only well above room temperature, rendering them unsuitable as solid-state electrolytes in energy-storage devices that typically operate at close to room temperature. To unlock their technological potential, strategies are needed to stabilize these superionic properties down to subambient temperatures. One such strategy involves altering the bulk properties by confinement within nanoporous insulators. In the current study, the unique structural and ion dynamical properties of an exemplary salt, NaCB11H12, nanodispersed within porous, high-surface-area silica via salt-solution infiltration were studied by differential scanning calorimetry, X-ray powder diffraction, neutron vibrational spectroscopy, nuclear magnetic resonance, quasielastic neutron scattering, and impedance spectroscopy. Combined results hint at the formation of a nanoconfined phase that is reminiscent of the high-temperature superionic phase of bulk NaCB11H12, with dynamically disordered CB11H12–anions exhibiting liquid-like reorientational mobilities. However, in contrast to this high-temperature bulk phase, the nanoconfined NaCB11H12phase with rotationally fluid anions persists down to cryogenic temperatures. Moreover, the high anion mobilities promoted fast-cation diffusion, yielding Na+superionic conductivities of ∼0.3 mS/cm at room temperature, with higher values likely attainable via future optimization. It is expected that this successful strategy for conductivity enhancement could be applied as well to other related polyhedral (carba)borate-based salts. Thus, these results present a new route to effectively utilize these types of superionic salts as solid-state electrolytes in future battery applications.

Published
2021
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29. NMR Studies of Lithium Diffusion in Li3(NH2)2I over Wide Range of Li+ Jump Rates

Author

Skripov, Alexander V., Volgmann, Kai, Chandran, C. Vinod, Skoryunov, Roman V., Babanova, Olga A., Soloninin, Alexei V., Orimo, Shin-Ichi, and Heitjans, Paul

Subjects
Dewey Decimal Classification::500 | Naturwissenschaften::540 | Chemie, nuclear magnetic resonance, ddc:540, spin-alignment echo, ddc:530, ion diffusion, spin-lattice relaxation, Dewey Decimal Classification::500 | Naturwissenschaften::530 | Physik, complex hydride
Abstract

We have studied the Li diffusion in the complex hydride Li3(NH2)2I which appears to exhibit fast Li ion conduction. To get a detailed insight into the Li motion, we have applied 7Li nuclear magnetic resonance spectroscopy methods, such as spin-lattice relaxation in the laboratory and rotating frames of reference, as well as spin-alignment echo. This combined approach allows us to probe Li jump rates over the wide dynamic range (~102–109 s−1). The spin-lattice relaxation data in the range 210–410 K can be interpreted in terms of a thermally-activated Li jump process with a certain distribution of activation energies. However, the low-temperature spin-alignment echo decays at T≤200 K suggest the presence of another Li jump process with the very low effective activation energy. © 2017 Walter de Gruyter GmbH, Berlin/Boston 2017.

Published
2017

31. Nature of Decahydro-closo-decaborate Anion Reorientations in an Ordered Alkali-Metal Salt: Rb2B10H10

Author

Dimitrievska, Mirjana, primary, Stavila, Vitalie, additional, Soloninin, Alexei V., additional, Skoryunov, Roman V., additional, Babanova, Olga A., additional, Wu, Hui, additional, Zhou, Wei, additional, Tang, Wan Si, additional, Faraone, Antonio, additional, Tarver, Jacob D., additional, Trump, Benjamin A., additional, Skripov, Alexander V., additional, and Udovic, Terrence J., additional

Published
2018
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33. Hydrogen dynamics in novel complex hydrides (poster)

Author

UCL - SST/IMCN/MOST - Molecules, Solids and Reactivity, Babanova, O. A., Skoryunov, R. V., Soloninin, A. V., Morelle, Fabrice, Skripov, A. V., Filinchuk, Yaroslav, Gordon Research Conference (GRC) on Hydrogen-Metal Systems, UCL - SST/IMCN/MOST - Molecules, Solids and Reactivity, Babanova, O. A., Skoryunov, R. V., Soloninin, A. V., Morelle, Fabrice, Skripov, A. V., Filinchuk, Yaroslav, and Gordon Research Conference (GRC) on Hydrogen-Metal Systems

Published
2017

34. Ultrafast H motion in lithium benzoimidozolate-borohydride Li2(bIm)(BH4) (poster)

Author

UCL - SST/IMCN/MOST - Molecules, Solids and Reactivity, Skripov, A. V., Soloninin, A. V., Babanova, O. A., Skoryunov, R. V., Morelle, Fabrice, Filinchuk, Yaroslav, Dimitrievska, M., Zhou, W., Udovic, T. J., Gordon Research Conference (GRC) on Hydrogen-Metal Systems, UCL - SST/IMCN/MOST - Molecules, Solids and Reactivity, Skripov, A. V., Soloninin, A. V., Babanova, O. A., Skoryunov, R. V., Morelle, Fabrice, Filinchuk, Yaroslav, Dimitrievska, M., Zhou, W., Udovic, T. J., and Gordon Research Conference (GRC) on Hydrogen-Metal Systems

Published
2017

38. Liquid-like Ionic Conduction in Solid Lithium and Sodium Monocarba-closo -decaborates near or at Room Temperature

Author

Tang, Wan Si, primary, Matsuo, Motoaki, additional, Wu, Hui, additional, Stavila, Vitalie, additional, Zhou, Wei, additional, Talin, A. Alec, additional, Soloninin, Alexei V., additional, Skoryunov, Roman V., additional, Babanova, Olga A., additional, Skripov, Alexander V., additional, Unemoto, Atsushi, additional, Orimo, Shin-ichi, additional, and Udovic, Terrence J., additional

Published
2016
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40. Comparison of Anion Reorientational Dynamics in MCB9H10and M2B10H10(M = Li, Na) via Nuclear Magnetic Resonance and Quasielastic Neutron Scattering Studies

Author

Soloninin, Alexei V., Dimitrievska, Mirjana, Skoryunov, Roman V., Babanova, Olga A., Skripov, Alexander V., Tang, Wan Si, Stavila, Vitalie, Orimo, Shin-ichi, and Udovic, Terrence J.

Abstract

The disordered phases of the 1-carba-closo-decaborates LiCB9H10and NaCB9H10exhibit the best solid-state ionic conductivities to date among all known polycrystalline competitors, likely facilitated in part by the highly orientationally mobile CB9H10–anions. We have undertaken both NMR and quasielastic neutron scattering (QENS) measurements to help characterize the monovalent anion reorientational mobilities and mechanisms associated with these two compounds and to compare their anion reorientational behaviors with those for the divalent B10H102–anions in the related Li2B10H10and Na2B10H10compounds. NMR data show that the transition from the low-Tordered to the high-Tdisordered phase for both LiCB9H10and NaCB9H10is accompanied by a nearly two-orders-of-magnitude increase in the reorientational jump rate of CB9H10–anions. QENS measurements of the various disordered compounds indicate anion jump correlation frequencies on the order of 1010–1011s–1and confirm that NaCB9H10displays jump frequencies about 60% to 120% higher than those for LiCB9H10and Na2B10H10at comparable temperatures. The Q-dependent quasielastic scattering suggests similar small-angular-jump reorientational mechanisms for the different disordered anions, changing from more uniaxial in character at lower temperatures to more multidimensional at higher temperatures, although still falling short of full three-dimensional rotational diffusion below 500 K within the nanosecond neutron window.

Published
2024
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41. Reorientational Motion in Alkali-Metal Borohydrides: NMR Data for RbBH4and CsBH4and Systematics of the Activation Energy Variations

Author

Babanova, Olga A., Soloninin, Alexei V., Skripov, Alexander V., Ravnsbæk, Dorthe B., Jensen, Torben R., and Filinchuk, Yaroslav

Abstract

To study the reorientational motion of the BH4groups in RbBH4and CsBH4, we have performed nuclear magnetic resonance (NMR) measurements of the 1H and 11B spin–lattice relaxation rates in these compounds over wide ranges of temperature (48–400 K) and resonance frequency (14–90 MHz). It is found that at low temperatures the reorientational motion in CsBH4is the fastest among all of the borohydrides studied so far. The activation energies Eafor BH4reorientations obtained from our data are 138 ± 4 meV for RbBH4and 105 ± 7 meV for CsBH4. Investigating the systematics of Eavariations in alkali-metal borohydrides MBH4, we have found a correlation between Eaand the relative deviation of the actual M–B distance from the sum of the ionic radii of M and BH4.

Published
2024
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46. NMR Studies of Lithium Diffusion in Li3(NH2)2I Over Wide Range of Li+ Jump Rates.

Author

Skripov, Alexander V., Volgmann, Kai, Chandran, C. Vinod, Skoryunov, Roman V., Babanova, Olga A., Soloninin, Alexei V., Orimo, Shin-ichi, and Heitjans, Paul

Subjects
LITHIUM ions, NUCLEAR magnetic resonance spectroscopy, SPIN-lattice relaxation
Abstract

We have studied the Li diffusion in the complex hydride Li3(NH2)2I which appears to exhibit fast Li ion conduction. To get a detailed insight into the Li motion, we have applied 7Li nuclear magnetic resonance spectroscopy methods, such as spin-lattice relaxation in the laboratory and rotating frames of reference, as well as spin-alignment echo. This combined approach allows us to probe Li jump rates over the wide dynamic range (~102-109 s−1). The spin-lattice relaxation data in the range 210-410 K can be interpreted in terms of a thermally-activated Li jump process with a certain distribution of activation energies. However, the low-temperature spin-alignment echo decays at T≤200 K suggest the presence of another Li jump process with the very low effective activation energy. [ABSTRACT FROM AUTHOR]

Published
2017
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47. Exceptional Superionic Conductivity in Disordered Sodium Decahydro-closo-decaborate

Author

Udovic, Terrence J., primary, Matsuo, Motoaki, additional, Tang, Wan Si, additional, Wu, Hui, additional, Stavila, Vitalie, additional, Soloninin, Alexei V., additional, Skoryunov, Roman V., additional, Babanova, Olga A., additional, Skripov, Alexander V., additional, Rush, John J., additional, Unemoto, Atsushi, additional, Takamura, Hitoshi, additional, and Orimo, Shin-ichi, additional

Published
2014
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