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3. Anomalous Impact of Mechanochemical Treatment on the Na-ion Conductivity of Sodium Closo-Carbadodecaborate Probed by X-Ray Raman Scattering Spectroscopy

Author

Gulino, Valerio, Longo, Alessandro, de Kort, Laura M., Rodenburg, Hendrik P., Murgia, Fabrizio, Brighi, Matteo, Černý, Radovan, Sahle, Christoph J., Sundermann, Martin, Gretarsson, Hlynur, de Groot, Frank, Ngene, Peter, Gulino, Valerio, Longo, Alessandro, de Kort, Laura M., Rodenburg, Hendrik P., Murgia, Fabrizio, Brighi, Matteo, Černý, Radovan, Sahle, Christoph J., Sundermann, Martin, Gretarsson, Hlynur, de Groot, Frank, and Ngene, Peter

Abstract

Solid-state sodium ion conductors are crucial for the next generation of all-solid-state sodium batteries with high capacity, low cost, and improved safety. Sodium closo-carbadodecaborate (NaCB11H12) is an attractive Na-ion conductor owing to its high thermal, electrochemical, and interfacial stability. Mechanical milling has recently been shown to increase conductivity by five orders of magnitude at room temperature, making it appealing for application in all-solid-state sodium batteries. Intriguingly, milling longer than 2 h led to a significant decrease in conductivity. In this study, X-ray Raman scattering (XRS) spectroscopy is used to probe the origin of the anomalous impact of mechanical treatment on the ionic conductivity of NaCB11H12. The B, C, and Na K-edge XRS spectra are successfully measured for the first time, and ab initio calculations are employed to interpret the results. The experimental and computational results reveal that the decrease in ionic conductivity upon prolonged milling is due to the increased proximity of Na to the CB11H12 cage, caused by severe distortion of the long-range structure. Overall, this work demonstrates how the XRS technique, allowing investigation of low Z elements such as C and B in the bulk, can be used to acquire valuable information on the electronic structure of solid electrolytes and battery materials in general.

Published
2024

4. Anomalous Impact of Mechanochemical Treatment on the Na-ion Conductivity of Sodium Closo-Carbadodecaborate Probed by X-Ray Raman Scattering Spectroscopy

Author

Sub Materials Chemistry and Catalysis, Materials Chemistry and Catalysis, Gulino, Valerio, Longo, Alessandro, de Kort, Laura M., Rodenburg, Hendrik P., Murgia, Fabrizio, Brighi, Matteo, Černý, Radovan, Sahle, Christoph J., Sundermann, Martin, Gretarsson, Hlynur, de Groot, Frank, Ngene, Peter, Sub Materials Chemistry and Catalysis, Materials Chemistry and Catalysis, Gulino, Valerio, Longo, Alessandro, de Kort, Laura M., Rodenburg, Hendrik P., Murgia, Fabrizio, Brighi, Matteo, Černý, Radovan, Sahle, Christoph J., Sundermann, Martin, Gretarsson, Hlynur, de Groot, Frank, and Ngene, Peter

Published
2024

6. Anomalous Impact of Mechanochemical Treatment on the Na‐ion Conductivity of Sodium Closo‐Carbadodecaborate Probed by X‐Ray Raman Scattering Spectroscopy

Author

Gulino, Valerio, primary, Longo, Alessandro, additional, de Kort, Laura M., additional, Rodenburg, Hendrik P., additional, Murgia, Fabrizio, additional, Brighi, Matteo, additional, Černý, Radovan, additional, Sahle, Christoph J., additional, Sundermann, Martin, additional, Gretarsson, Hlynur, additional, de Groot, Frank, additional, and Ngene, Peter, additional

Published
2023
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7. Thermal Polymorphism in CsCB11H12

Author

Černý, Radovan, Brighi, Matteo, Wu, Hui, Zhou, Wei, Dimitrievska, Mirjana, Murgia, Fabrizio, Gulino, Valerio, de Jongh, Petra E., Trump, Benjamin A., Udovic, Terrence J., Černý, Radovan, Brighi, Matteo, Wu, Hui, Zhou, Wei, Dimitrievska, Mirjana, Murgia, Fabrizio, Gulino, Valerio, de Jongh, Petra E., Trump, Benjamin A., and Udovic, Terrence J.

Abstract

Thermal polymorphism in the alkali-metal salts incorporating the icosohedral monocarba-hydridoborate anion, CB11H12−, results in intriguing dynamical properties leading to superionic conductivity for the lightest alkali-metal analogues, LiCB11H12 and NaCB11H12. As such, these two have been the focus of most recent CB11H12− related studies, with less attention paid to the heavier alkali-metal salts, such as CsCB11H12. Nonetheless, it is of fundamental importance to compare the nature of the structural arrangements and interactions across the entire alkali-metal series. Thermal polymorphism in CsCB11H12 was investigated using a combination of techniques: X-ray powder diffraction; differential scanning calorimetry; Raman, infrared, and neutron spectroscopies; and ab initio calculations. The unexpected temperature-dependent structural behavior of anhydrous CsCB11H12 can be potentially justified assuming the existence of two polymorphs with similar free energies at room temperature: (i) a previously reported, ordered R3 polymorph stabilized upon drying and transforming first to R3c symmetry near 313 K and then to a similarly packed but disordered I43d polymorph near 353 K and (ii) a disordered Fm3 polymorph that initially appears from the disordered I43d polymorph near 513 K along with another disordered high-temperature P63mc polymorph. Quasielastic neutron scattering results indicate that the CB11H12− anions in the disordered phase at 560 K are undergoing isotropic rotational diffusion, with a jump correlation frequency [1.19(9) × 1011 s−1] in line with those for the lighter-metal analogues.

Published
2023

8. Thermal Polymorphism in CsCB11H12

Author

Sub Materials Chemistry and Catalysis, Materials Chemistry and Catalysis, Černý, Radovan, Brighi, Matteo, Wu, Hui, Zhou, Wei, Dimitrievska, Mirjana, Murgia, Fabrizio, Gulino, Valerio, de Jongh, Petra E., Trump, Benjamin A., Udovic, Terrence J., Sub Materials Chemistry and Catalysis, Materials Chemistry and Catalysis, Černý, Radovan, Brighi, Matteo, Wu, Hui, Zhou, Wei, Dimitrievska, Mirjana, Murgia, Fabrizio, Gulino, Valerio, de Jongh, Petra E., Trump, Benjamin A., and Udovic, Terrence J.

Published
2023

9. Thermal Polymorphism in CsCB11H12

Author

Černý, Radovan, primary, Brighi, Matteo, additional, Wu, Hui, additional, Zhou, Wei, additional, Dimitrievska, Mirjana, additional, Murgia, Fabrizio, additional, Gulino, Valerio, additional, de Jongh, Petra E., additional, Trump, Benjamin A., additional, and Udovic, Terrence J., additional

Published
2023
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17. Enhanced Room-Temperature Ionic Conductivity of NaCB11H12via High-Energy Mechanical Milling

Author

Murgia, Fabrizio, Brighi, Matteo, Piveteau, Laura, Avalos, Claudia E., Gulino, Valerio, Nierstenhöfer, Marc C., Ngene, Peter, De Jongh, Petra, Černý, Radovan, Murgia, Fabrizio, Brighi, Matteo, Piveteau, Laura, Avalos, Claudia E., Gulino, Valerio, Nierstenhöfer, Marc C., Ngene, Peter, De Jongh, Petra, and Černý, Radovan

Abstract

The body-centered cubic (bcc) polymorph of NaCB11H12 has been stabilized at room temperature by high-energy mechanical milling. Temperature-dependent electrochemical impedance spectroscopy shows an optimum at 45-min milling time, leading to an rt conductivity of 4 mS cm-1. Mechanical milling suppresses an order-disorder phase transition in the investigated temperature range. Nevertheless, two main regimes can be identified, with two clearly distinct activation energies. Powder X-ray diffraction and 23Na solid-state NMR reveal two different Na+ environments, which are partially occupied, in the bcc polymorph. The increased number of available sodium sites w.r.t. ccp polymorph raises the configurational entropy of the bcc phase, contributing to a higher ionic conductivity. Mechanical treatment does not alter the oxidative stability of NaCB11H12. Electrochemical test on a symmetric cell (Na|NaCB11H12|Na) without control of the stack pressure provides a critical current density of 0.12 mA cm-2, able to fully charge/discharge a 120 mA h g-1 specific capacity positive electrode at the rate of C/2.

Published
2021

18. Room-Temperature Solid-State Lithium-Ion Battery Using a LiBH4-MgO Composite Electrolyte

Author

Gulino, Valerio, Brighi, Matteo, Murgia, Fabrizio, Ngene, Peter, De Jongh, Petra, Černý, Radovan, Baricco, Marcello, Gulino, Valerio, Brighi, Matteo, Murgia, Fabrizio, Ngene, Peter, De Jongh, Petra, Černý, Radovan, and Baricco, Marcello

Abstract

LiBH4 has been widely studied as a solid-state electrolyte in Li-ion batteries working at 120 °C due to the low ionic conductivity at room temperature. In this work, by mixing with MgO, the Li-ion conductivity of LiBH4 has been improved. The optimum composition of the mixture is 53 v/v % of MgO, showing a Li-ion conductivity of 2.86 × 10-4 S cm-1 at 20 °C. The formation of the composite does not affect the electrochemical stability window, which is similar to that of pure LiBH4 (about 2.2 V vs Li+/Li). The mixture has been incorporated as the electrolyte in a TiS2/Li all-solid-state Li-ion battery. A test at room temperature showed that only five cycles already resulted in cell failure. On the other hand, it was possible to form a stable solid electrolyte interphase by applying several charge/discharge cycles at 60 °C. Afterward, the battery worked at room temperature for up to 30 cycles with a capacity retention of about 80%.

Published
2021

19. Room-Temperature Solid-State Lithium-Ion Battery Using a LiBH4-MgO Composite Electrolyte

Author

Sub Materials Chemistry and Catalysis, Materials Chemistry and Catalysis, Gulino, Valerio, Brighi, Matteo, Murgia, Fabrizio, Ngene, Peter, De Jongh, Petra, Černý, Radovan, Baricco, Marcello, Sub Materials Chemistry and Catalysis, Materials Chemistry and Catalysis, Gulino, Valerio, Brighi, Matteo, Murgia, Fabrizio, Ngene, Peter, De Jongh, Petra, Černý, Radovan, and Baricco, Marcello

Published
2021

21. Erratum: Hadjixenophontos, E.; et al. A Review of the MSCA ITN ECOSTORE—Novel Complex Metal Hydrides for Efficient and Compact Storage of Renewable Energy as Hydrogen and Electricity. Inorganics 2020, 8, 17

Author

Hadjixenophontos, Efi, primary, Dematteis, Erika Michela, additional, Berti, Nicola, additional, Wołczyk, Anna Roza, additional, Huen, Priscilla, additional, Brighi, Matteo, additional, Le, Thi Thu, additional, Santoru, Antonio, additional, Payandeh, SeyedHosein, additional, Peru, Filippo, additional, Dao, Anh Ha, additional, Liu, Yinzhe, additional, and Heere, Michael, additional

Published
2020
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25. A Review of the MSCA ITN ECOSTORE—Novel Complex Metal Hydrides for Efficient and Compact Storage of Renewable Energy as Hydrogen and Electricity

Author

Hadjixenophontos, Efi, primary, Dematteis, Erika Michela, additional, Berti, Nicola, additional, Wołczyk, Anna Roza, additional, Huen, Priscilla, additional, Brighi, Matteo, additional, Le, Thi Thu, additional, Santoru, Antonio, additional, Payandeh, SeyedHosein, additional, Peru, Filippo, additional, Dao, Anh Ha, additional, Liu, Yinzhe, additional, and Heere, Michael, additional

Published
2020
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27. Metal hydroborates as solid electrolyte for Li- and Na-ion batteries

Author

Brighi, Matteo and Cerny, Radovan

Subjects
Borohydride, Ionic conductivity, Powder diffraction, Solid Electrolyte, Closoborates, ddc:500.2, Na-ion conductors, Na-batteries
Abstract

This thesis focuses on the development of novel solid electrolyte suitable for Li and post-lithium batteries. Novel hydroborates are proposed as potential candidate for this role. The understanding of their structures, characterized by X-ray diffraction, was necessary to understand the ionic mobility and to make possible the developments of strategies to stabilize conducting phases at room temperature. The best results were obtained within the closoborates, by means of anion mixing, where the ionic conductivity exceeds 1 mS/cm already at room temperature (a very competitive value compared to the conventional liquid electrolytes). The best performing ionic conductors where hence characterized in electrochemical cells to understand possible kinetic and compatibility limitations with respect to different electrodes: sodium, tin and indium were selected as anode materials, showing in the best cases (In) a reversible Na-shuttling for more than 2000 hours.

Published
2018

31. Insights into the Rb–Mg–N–H System: an Ordered Mixed Amide/Imide Phase and a Disordered Amide/Hydride Solid Solution

Author

Santoru, Antonio, primary, Pistidda, Claudio, additional, Brighi, Matteo, additional, Chierotti, Michele R., additional, Heere, Michael, additional, Karimi, Fahim, additional, Cao, Hujun, additional, Capurso, Giovanni, additional, Chaudhary, Anna-Lisa, additional, Gizer, Gökhan, additional, Garroni, Sebastiano, additional, Sørby, Magnus H., additional, Hauback, Bjørn C., additional, Černý, Radovan, additional, Klassen, Thomas, additional, and Dornheim, Martin, additional

Published
2018
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35. Li5(BH4)3NH: Lithium-Rich Mixed Anion Complex Hydride

Author

Wolczyk, Anna, primary, Paik, Biswajit, additional, Sato, Toyoto, additional, Nervi, Carlo, additional, Brighi, Matteo, additional, GharibDoust, SeyedHosein Payandeh, additional, Chierotti, Michele, additional, Matsuo, Motoaki, additional, Li, Guanqiao, additional, Gobetto, Roberto, additional, Jensen, Torben R., additional, Černý, Radovan, additional, Orimo, Shin-ichi, additional, and Baricco, Marcello, additional

Published
2017
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42. Phase Stability and Fast Ion Conductivity in the Hexagonal LiBH4–LiBr–LiCl Solid Solution

Author

Gulino, Valerio, Brighi, Matteo, Dematteis, Erika M., Murgia, Fabrizio, Nervi, Carlo, Černý, Radovan, and Baricco, Marcello

Abstract

This study shows a flexible system that offers promising candidates for Li-based solid-state electrolytes. The Br–substitution for BH4–stabilizes the hexagonal structure of LiBH4at room temperature (RT), whereas Cl–is soluble only at higher temperatures. Incorporation of chloride in a hexagonal solid solution leads to an increase in the energy density of the system. For the first time, a stable hexagonal solid solution of LiBH4containing both Cl–and Br-halide anions has been obtained at RT. The LiBH4–LiBr–LiCl ternary phase diagram has been determined at RT by X-ray diffraction coupled with a Rietveld refinement. A solubility of up to 30% of Cl–in the solid solution has been established. The effect of halogenation on the Li-ion conductivity and electrochemical stability has been investigated by electrochemical impedance spectroscopy and cyclic voltammetry. Considering the ternary samples, h-Li(BH4)0.7(Br)0.2(Cl)0.1composition showed the highest value for conductivity (1.3 × 10–5S/cm at 30 °C), which is about 3 orders of magnitude higher than that for pure LiBH4in the orthorhombic structure. The values of Li-ion conductivity at RT depend only on the BH4–content in the solid solution, suggesting that the Br/Cl ratio does not affect the defect formation energy in the structure. Chloride anion substitution in the hexagonal structure increases the activation energy, moving from about 0.45 eV for samples without Cl–ions in the structure up to about 0.63 eV for h-Li(BH4)0.6(Br)0.2(Cl)0.2compositions, according to the Meyer–Neldel rule. In addition to increasing Li-ion conductivity, the halogenation also increases the thermal stability of the system. Unlike for the Li-ion conductivity, the Br/Cl ratio influences the electrochemical stability: a wide oxidative window of 4.04 V versus Li+/Li is reached in the Li–Br system while further addition of Cl is a trade-off between oxidative stability and weight reduction. The halogenation allows both binary and ternary systems operating below 120 °C, thus suggesting possible applications of these fast ion conductors as solid-state electrolytes in Li-ion batteries.

Published
2024
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47. Hydrogen Sorption in Erbium Borohydride Composite Mixtures with LiBH4 and/or LiH.

Author

Heere, Michael, GharibDoust, Seyed Hosein Payandeh, Brighi, Matteo, Frommen, Christoph, Sørby, Magnus H., ???erný, Radovan, Jensen, Torben R., and Hauback, Bjørn C.

Subjects
HYDROGEN storage, ERBIUM, BOROHYDRIDE, SORPTION, CHEMICAL decomposition, RARE earth metals, METAL complexes
Abstract

Rare earth (RE) metal borohydrides have recently been receiving attention as possible hydrogen storage materials and solid-state Li-ion conductors. In this paper, the decomposition and reabsorption of Er(BH4)3 in composite mixtures with LiBH4 and/or LiH were investigated. The composite of 3LiBH4 + Er(BH4)3 + 3LiH has a theoretical hydrogen storage capacity of 9 wt %, nevertheless, only 6 wt % hydrogen are accessible due to the formation of thermally stable LiH. Hydrogen sorption measurements in a Sieverts-type apparatus revealed that during three desorption-absorption cycles of 3LiBH4 + Er(BH4)3 + 3LiH, the composite desorbed 4.2, 3.7 and 3.5 wt % H for the first, second and third cycle, respectively, and thus showed good rehydrogenation behavior. In situ synchrotron radiation powder X-ray diffraction (SR-PXD) after ball milling of Er(BH4)3 + 6LiH resulted in the formation of LiBH4, revealing that metathesis reactions occurred during milling in these systems. Impedance spectroscopy of absorbed Er(BH4)3 + 6LiH showed an exceptional high hysteresis of 40-60 K for the transition between the high and low temperature phases of LiBH4, indicating that the high temperature phase of LiBH4 is stabilized in the composite. [ABSTRACT FROM AUTHOR]

Published
2017
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48. Superionic Conduction of Sodium and Lithium in Anion-Mixed Hydroborates Na3BH4B12H12 and (Li0.7Na0.3)3BH4B12H12.

Author

Sadikin, Yolanda, Brighi, Matteo, Schouwink, Pascal, and Černý, Radovan

Subjects
*SODIUM, *LITHIUM, *HYDROBORATION, *COVALENT bonds, *BALL mills, *METAL borohydrides, *CATIONS, *CRYSTAL structure
Abstract

Novel mixed‐anion compounds Na3BH4B12H12 and (Li0.7Na0.3)3BH4B12H12 show superionic conduction corresponding to highly disordered cations and continuous migration paths in the structure. Na‐rich Na3BH4B12H12 with a room‐temperature conductivity of 0.5 × 10−3 S cm−1 provides a light‐weight solution for the electrolyte in Na‐based, all solid‐state batteries. (Li0.7Na0.3)3BH4B12H12 favors ionic conductivity for both Li and Na cations, but only above 500 K. [ABSTRACT FROM AUTHOR]

Published
2015
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49. Superionic Conduction of Sodium and Lithium in Anion-Mixed Hydroborates Na3BH4B12H12 and (Li0.7Na0.3)3BH4B12H12.

Author

Sadikin, Yolanda, Brighi, Matteo, Schouwink, Pascal, and Černý, Radovan

Subjects
SODIUM, LITHIUM, HYDROBORATION, COVALENT bonds, BALL mills, METAL borohydrides, CATIONS, CRYSTAL structure
Abstract

Novel mixed‐anion compounds Na3BH4B12H12 and (Li0.7Na0.3)3BH4B12H12 show superionic conduction corresponding to highly disordered cations and continuous migration paths in the structure. Na‐rich Na3BH4B12H12 with a room‐temperature conductivity of 0.5 × 10−3 S cm−1 provides a light‐weight solution for the electrolyte in Na‐based, all solid‐state batteries. (Li0.7Na0.3)3BH4B12H12 favors ionic conductivity for both Li and Na cations, but only above 500 K. [ABSTRACT FROM AUTHOR]

Published
2015
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50. Anion Disorder in K3BH4B12H12and Its Effect on Cation Mobility

Author

Sadikin, Yolanda, Skoryunov, Roman V., Babanova, Olga A., Soloninin, Alexei V., Lodziana, Zbigniew, Brighi, Matteo, Skripov, Alexander V., and Černý, Radovan

Abstract

Mixed anion borohydride, closo-borane of potassium, K3BH4B12H12, has been synthesized using mechanochemistry and characterized by combination of temperature dependent synchrotron radiation X-ray powder diffraction, solid state nuclear magnetic resonance, thermal analysis, electrochemical impedance spectroscopy, topology analysis, and ab initio solid state calculations. At RT the compound crystallizes in the monoclinic superstructure (P2/c) of the cubic antiperovskite prototype. At 565 K it transforms by first order phase transition into a rhombohedral (R-3m) deformation of the cubic prototype, which further transforms at 680 K by a second order phase transition into a cubic (P23) antiperovskite structure. While the monoclinic polymorph is observed for the first time among mixed anion salts, the rhombohedral and cubic polymorphs are known among other alkali metal and ammonium halides (or borohydrides), closo-boranes. The first phase transition is related to the repulsive homopolar H–H contacts between BH4–and B12H122–anions which are released at bigger cell volumes, and the orientation of BH4–anion becomes disordered. The second phase transition is related to orientational disorder of the B12H122–anion at bigger cell volumes. The parameters of reorientational motion (activation energies and jump rates) for both BH4–and B12H122–anions in the monoclinic phase were found from the nuclear spin–lattice relaxation measurements. The effect of orientation disorder of both anions on mobility of cations was studied as a case example for the whole family of complex hydrides based on borohydride or closo-borane anions, important solid state electrolytes. While the dynamics of smaller BH4–anion does not have any measurable effect on K+mobility, the dynamics and orientation disorder of bigger B12H122–is promoting the K+mobility which would otherwise be limited by the small radius of conducting channels even in the cubic antiperovskite structure.

Published
2017
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