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Instruments / Technical Area	Publication Details	Published
I09-Surface and Interface Structural Analysis	Effect of current density on the solid electrolyte interphase formation at the lithium∣Li6PS5Cl interface Sudarshan Narayanan , Ulderico Ulissi , Joshua S. Gibson , Yvonne A. Chart , Robert S Weatherup , Mauro Pasta Nature Communications 13 DOI: 10.1038/s41467-022-34855-9 Diamond Proposal Number(s): [25807] Open Access Show Abstract ▼ Abstract: Understanding the chemical composition and morphological evolution of the solid electrolyte interphase (SEI) formed at the interface between the lithium metal electrode and an inorganic solid-state electrolyte is crucial for developing reliable all-solid-state lithium batteries. To better understand the interaction between these cell components, we carry out X-ray photoemission spectroscopy (XPS) measurements during lithium plating on the surface of a Li6PS5Cl solid-state electrolyte pellet using an electron beam. The analyses of the XPS data highlight the role of Li plating current density on the evolution of a uniform and ionically conductive (i.e., Li3P-rich) SEI capable of decreasing the electrode∣solid electrolyte interfacial resistance. The XPS findings are validated via electrochemical impedance spectrsocopy measurements of all-solid-state lithium-based cells.	Nov 2022
I09-Surface and Interface Structural Analysis	Gently does it!: in situ preparation of alkali metal - solid electrolyte interfaces for photoelectron spectroscopy Joshua Gibson , Sudarshan Narayanan , Jack E. N. Swallow , Pardeep K. Thakur , Mauro Pasta , Tien-Lin Lee , Robert S. Weatherup Faraday Discussions DOI: 10.1039/D1FD00118C Diamond Proposal Number(s): [25807] Show Abstract ▼ Abstract: The key charge transfer processes in energy storage devices occur at the electrode-electrolyte interface, which is typically buried making it challenging to access the interfacial chemistry. In the case of Li-ion batteries, metallic Li electrodes hold promise for increasing energy and power densities, and when used in conjunction with solid electrolytes adverse safety implications associated with dendrite formation in organic liquid electrolytes can potentially be overcome. To better understand the stability of solid electrolytes when in contact with alkali metals and the reactions that occur, here we consider the deposition of thin (~10 nm) alkali metal films onto solid electrolyte surfaces, that are thin enough that X-ray photoelectron spectroscopy can probe the buried electrode-electrolyte interface. We highlight the importance of in situ alkali metal deposition, by assessing the contaminant species that are present after glovebox handling and the use of ‘inert’ transfer devices. Consequently, we compare and contrast three available methods for in situ alkali-metal deposition; Li sputter deposition, Li evaporation, and Li plating induced by e− flood-gun irradiation. Studies on both a sulphide solid electrolyte (Li6PS5Cl), and a single-layer graphene probe surface reveal that the more energetic Li deposition methods such as sputtering can induce surface damage and interfacial mixing that is not seen with thermal evaporation. This indicates that appropriate selection of the Li deposition method for in situ studies is required to observe representative behaviour, and the results of previous studies involving energetic deposition may warrant further evaluation.	Jan 2022
I09-Surface and Interface Structural Analysis	Thin film structural analysis using variable-period x-ray standing waves Joshua S. Gibson , Karen L. Syres , Matthew Buckley , Tien-Lin Lee , Pardeep K. Thakur , Robert G. Jones Physical Review B 98, 165402 DOI: 10.1103/PhysRevB.98.165402 Diamond Proposal Number(s): [9118] Show Abstract ▼ Abstract: Variable-period x-ray standing wave (VPXSW) studies have been carried out using 3 keV x rays and photoelectron detection. Two model surfaces have been used, a native SiO2 layer (20 Å thick) on bulk silicon, and a purpose-built multilayer surface comprising a chloroform/water marker layer (12 Å thick) on an ionic liquid spacer layer (211 Å thick) deposited on a SiO2/Si substrate at 90 K. By using photoelectron detection, both chemical and elemental sensitivity were achieved. The surfaces were modeled using dynamic x-ray scattering for x-ray intensity, and attenuation of photoelectrons transmitted through the layers, to produce simulations which accurately reproduced the experimental VPXSW measurements. VPXSW measurements made using the substrate, spacer layer, and marker layer photoelectron signatures produced consistent structural values. This work demonstrates that VPXSW can be used to determine chemically specific layer thicknesses within thick (300 Å) surface structures composed of the light elements B, C, N, O, F, and Cl with an accuracy of 10 to 15 Å, perpendicular to the surface.	Oct 2018

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