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Instruments / Technical Area	Publication Details	Published
I09-Surface and Interface Structural Analysis	Investigation of electrolyte salts in non-flammable triethyl phosphate for sodium-ion batteries Wessel W. A. Van Ekeren , Lasse Dettmann , Yonas Tesfamhret , Andrew J. Naylor , Reza Younesi Batteries & Supercaps DOI: 10.1002/batt.202400489 Diamond Proposal Number(s): [36213] Open Access Show Abstract ▼ Abstract: Five different electrolyte salts, namely NaBF4, NaClO4, NaDFOB, NaFSI and NaPF6, were evaluated in non-flammable triethyl phosphate (TEP) based electrolyte solutions in sodium-ion full-cells using high-mass loading Prussian white and hard carbon electrodes. Their impact on the viscosity, ionic conductivity and solvation structure was analyzed, revealing that NaFSI-based electrolytes exhibited a stronger interaction with TEP and less ion-pairing than the other salts, resulting in the highest ionic conductivity at a concentration of 0.8 m (mol/kg). Galvanostatic cycling experiments showed that none of the electrolyte salts dissolved in TEP forms an efficient passivation layer. However, adding 1 wt.% vinylene carbonate (VC) significantly improved cycling performance for the cells with NaBF4, NaDFOB or NaFSI, but not with NaClO4 or NaPF6. Additionally, NaFSI in TEP with 1 wt.% VC electrolyte solution showed minimal gas evolution during the formation cycling (< 8 mbar). In a 1 Ah multilayer pouch cell, 0.8 m NaFSI in TEP with 1 wt.% VC showed promising results with 88% capacity retention after 200 cycles. X-ray photoelectron spectroscopy analysis revealed that the addition of VC results in the formation of a thin SEI and minimized TEP decomposition on hard carbon, especially for 0.8 m NaFSI TEP with 1 wt.% VC.	Oct 2024
I09-Surface and Interface Structural Analysis	Interfacial decomposition behaviour of triethyl phosphate-based electrolytes for lithium-ion batteries Florian Gebert , Robin Lundström , Wessel Van Ekeren , Andrew Naylor Batteries & Supercaps DOI: 10.1002/batt.202400342 Diamond Proposal Number(s): [31857] Open Access Show Abstract ▼ Abstract: Triethyl phosphate (TEP) is a cheap, environmentally benign, and non-flammable electrolyte solvent, whose implementation in lithium-ion batteries is held back by its co-intercalation into graphite anodes, resulting in exfoliation of the graphite structure. In this work, the electrode-electrolyte interface behaviour of electrolytes containing up to 100% TEP was investigated and correlated to electrochemical performance. High capacity and stable cycling are maintained with up to 30% TEP in carbonate ester-based electrolytes, but above this threshold the reversibility of Li+ intercalation into graphite drops sharply to almost zero. This represents a potential route to improved battery safety, while TEP can also improve safety indirectly by enabling the use of lithium bis(oxalato borate), a fluorine-free salt with limited solubility in traditional electrolytes. To understand the poor performance at TEP concentrations of >30%, its solvation behaviour and interfacial reaction chemistry were studied. Nuclear magnetic resonance spectroscopy data confirms changes in the Li+ solvation shell above 30% TEP, while operando gas analysis indicates extensive gas evolution from TEP decomposition at the electrode above the threshold concentration, which is almost entirely absent below it. X-ray photoelectron spectroscopy depth profiling of electrodes demonstrates poor passivation by the solid electrolyte interphase above 30% TEP and significant graphite exfoliation.	Jul 2024
I11-High Resolution Powder Diffraction	Layered titanium sulfide cathode for all-solid-state magnesium batteries Lasse N. Skov , Jakob B. Grinderslev , Torben R. Jensen Batteries & Supercaps DOI: 10.1002/batt.202300185 Open Access Show Abstract ▼ Abstract: Magnesium solid-state batteries attract significant attention as a future mean of energy storage. Here we present the first cathode study of an inorganic all-solid-state magnesium battery using a magnesium metal anode, a nanocomposite electrolyte Mg(BH4)2·1.6NH3-MgO(75 wt%), and a layered titanium disulfide (TiS2) as cathode active material. The structural transformations of TiS2 particles with different size are investigated at different stages of battery life. Reversible Mg2+ intercalation occurs via three structurally distinct phases of MgxTiS2, identified by powder X-ray diffraction. Magnesium intercalates initially on octahedral sites and at higher depth of discharge on tetrahedral sites in the interlayers of TiS2, which leads to an expansion initially mainly along the c-axis and later along both the a- and c-axes. A maximum discharge capacity of 172 mAh g-1 (Δx = 0.36 in MgxTiS2) is observed for smaller TiS2 particles. Parasitic reactions could be reduced by decreasing the cut-off voltage by a constant current constant voltage cycling procedure. The chemical diffusion coefficient of the entire cell is found from galvanostatic intermittent titration technique experiments to be in the order of 10-15 to 10-19 cm2 s-1.	Jun 2023
I11-High Resolution Powder Diffraction	Towards solid state magnesium batteries: ligand-assisted superionic conductivity Lasse N. Skov , Jakob B. Grinderslev , Asger Rosenkranz , Young-Su Lee , Torben R. Jensen Batteries & Supercaps DOI: 10.1002/batt.202200163 Diamond Proposal Number(s): [26090] Open Access Show Abstract ▼ Abstract: Solid-state inorganic magnesium batteries are considered as potential high energy storage devices for the future. Here we present a series of magnesium borohydride tetrahydrofuran (THF) composites, Mg(BH 4 ) 2 · x THF(−MgO), 0 ≤ x ≤ 3, as solid-state electrolytes for magnesium batteries. Three new monoclinic compounds were identified, Mg(BH 4 ) 2 ·2/3THF ( Cc ), α-Mg(BH 4 ) 2 ·2THF ( P2 1 /c ) and β-Mg(BH 4 ) 2 ·2THF ( C2 ), and the detailed structures of α− and β−Mg(BH 4 ) 2 ·2THF are presented. The magnesium ionic conductivity of composites formed by these compounds were several orders of magnitude higher than that of the distinct compounds, x = 0, 2/3, 2, and 3. The nanocomposite stabilized by MgO nanoparticles (~50 nm), Mg(BH 4 ) 2 ·1.5THF−MgO(75 wt%), displayed the highest Mg 2+ conductivity, σ(Mg 2+ ) ~10 -4 S cm -1 at 70 °C, a high ionic transport number of t ion = 0.99, and cyclic voltammetry revealed an oxidative stability of ~1.2 V vs. Mg/Mg 2+ . The electrolyte was stable towards magnesium electrodes, which allowed for stable Mg plating/stripping for at least 100 cycles at 55 °C with a current density of 0.1 mA cm -2 . Finally, a proof-of-concept rechargeable solid-state magnesium battery was assembled with a magnesium metal anode, a TiS 2 cathode providing a maximum discharge capacity of 94.2 mAh g -1 , which corresponds to y = 0.2 in Mg y TiS 2.	Jun 2022
I09-Surface and Interface Structural Analysis	Electrochemical utilization of iron IV in the Li1.3Fe0.4Nb0.3O2 disordered rocksalt cathode Zachary W. Lebens-Higgins , Hyeseung Chung , Israel Temprano , Mateusz Zuba , Jinpeng Wu , Jatinkumar Rana , Carlos Mejia , Michael A. Jones , Le Wang , Clare P. Grey , Yingge Du , Wanli Yang , Ying Shirley Meng , Louis F. J. Piper Batteries & Supercaps 144 DOI: 10.1002/batt.202000318 Diamond Proposal Number(s): [22250, 22148] Show Abstract ▼ Abstract: Interest in alkali‐rich oxide cathodes has grown in an effort to identify systems that provide high energy densities through reversible oxygen redox. However, some of the most promising compositions such as those based solely on earth abundant elements, e. g., iron and manganese, suffer from poor capacity retention and large hysteresis. Here, we use the disordered rocksalt cathode, Li1.3Fe0.4Nb0.3O2, as a model system to identify the underlying origin for the poor performance of Li‐rich iron‐based cathodes. Using elementally specific spectroscopic probes, we find the first charge is primarily accounted for by iron oxidation to 4+ below 4.25 V and O2 gas release beyond 4.25 V with no evidence of bulk oxygen redox. Although the Li1.3Fe0.4Nb0.3O2 is not a viable oxygen redox cathode, the iron 3+/4+ redox couple can be used reversibly during cycling.	Jan 2021

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