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Reviews ab 800 700 600 500 400 300 200 100 1st charge Irreversible 1st discharge 2nd charge Reversible 2nd discharge c S2p d Interfacial layer Li2S–P2S5 50 nm 0 3.0 3.2 3.4 3.6 3.4 3.2 3.0 3.0 3.2 3.4 3.6 3.4 3.2 3.0 1.0 1.5 LiCoO2 2.0 2.5 Voltage (V) Open-circuit voltage vs Li+/Li-In (V) 0.6 0.4 0.2 0 –0.2 –0.4 1st cycle 3.0 3.5 Before Charge Discharge 166 164 162 160 Binding energy (eV) Non-bridging S 158 S–S 100 80 60 40 20 0 Fig. 3 | (electro)chemical instability of sulfide solid electrolytes. a | Evolution of four components of the resistance in a Li-In|β-Li3PS4|NCM-811/β-Li4PS4 cell obtained by fitting the impedance spectra in the first and second cycles as a function of the open-circuit voltage. b | Cyclic voltammetry of a Li| Li10GeP2S12 (LGPS)|LGPS+C|Pt cell between 1.0 and 3.5 V. c | S2p X-ray photoelectron spectra of the Li3PS4 glass+carbon composite electrode before and after charge–discharge processes. d | Cross-sectional, high-angle, annular dark-field imaging scanning transmission electron microscope image of the LiCoO2 electrode/Li2S–P2S5 interface after the first charge (top) and cross-sectional energy-dispersive X-ray spectroscopy line profiles for Co, P and S (bottom). RSE,anode, interfacial resistance between the solid electrolyte and the anode; RSE,bulk, bulk resistance of the solid electrolyte; RSE,cathode, interfacial resistance between the solid electrolyte and the cathode; RSE,gb, grain boundary resistance of the solid electrolyte. Part a is reproduced with permission from ref.60, American Chemical Society. Part b is reproduced with permission from ref.98, Wiley-VCH. Part c is reproduced with permission from ref.102, American Chemical Society. Part d is reproduced with permission from ref.47, American Chemical Society. Oxidation products of sulfides Fairly good consistency between experimental and computational results has also been observed for the oxidation decomposition products of sulfide SEs. The predicted oxidation products for Li2S–P2S5 include elemental sulfur64–66 and more condensed sulfides with lower lithium content, such as P2S5 (refs65,66), Li4P2S6 and P2S7 (ref.64), as well as GeS2 for LGPS64–66. In exper- iments, P2S5 was not directly observed using XPS; however, oxidized sulfur species with S–S bonds have been detected at the LiNi0.8Co0.1Mn0.1O2/β-Li3PS4 inter- face60,68, possibly indicating the presence of elemental sulfur. Similar bridging of S–S bonds between PS4 groups has been observed at the Li3PS4 glass/carbon interface after charging to 3.6 V (ref.102). A β-Li3PS4+carbon cathode was charged to 5 V and the formation of ele- mental sulfur was observed103, further confirming that S2− in sulfide SEs oxidizes at high voltages. For LGPS, RSE, bulk RSE, gb RSE, cathode RSE, anode Co 0 20 40 60 80 100 Distance (nm) S P www.nature.com/natrevmats Content (atom %) Resistance (Ω) Current (mA)PDF Image | Understanding interface stability in solid-state batteries
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