Publication date: 10th April 2024
Conventional organic liquid electrolytes fall short in meeting the energy storage demand due to their limited chemical and electrochemical stability in lithium metal-based rechargeable batteries. To overcome these problems, solid electrolytes (SEs) appear as an innovative technological breakthrough in the energy storage field. Owing to their chemical composition and inherent structural rigidity, SEs provide higher energy and power densities and eliminate some of the concerning safety issues of liquid-based Li-ion batteries[1]. Sulphur-based solid electrolytes, Li6PS5X (X=Cl, Br), Li3PS4, Li10GeP2S12 and xLi2S-(1-x)P2S5 glass-ceramics are promising candidates for all-solid-state batteries due to their intrinsic physicochemical properties such as high lithium diffusion coefficient, low processing temperatures and low pressures needed to maintain good interfacial contact with cathode due to low young’s modulus[2].
However, a primary concern of sulphide electrolytes is the narrow electrochemical stability window and the undesired secondary (electro-)chemical reactions occurring at the interface with Li-metal anode[3]. The abovementioned sulphide SEs are thermodynamically unstable towards Li-metal, which lead to the formation of a mixed interphase (mainly Li2S and Li3P) with relatively poor Li-ion conducting properties. These reduced products increase heterogeneity at the Li/SE interface and lead to current focussing. This worsens void formation during stripping and further leads to nucleation spots for Li metal dendrite initiation[4]. Recently, a new family of solid electrolytes consisting of the fully reduced Li3P-Li2S and Li3N-LiCl solid solutions has been reported; exhibiting high ionic conductivity, low activation energy, and good thermodynamic stability against Li-metal[5], [6].
In the current study, we evaluate the electrochemical performance of Li3P-Li2S solid solution at room temperature and under controlled pressure in Li|Li symmetric cells. To evaluate the promising (electro-)chemical stability of the fully reduced Li8P2S SE with Li-metal anode, uni-directional Li plating-stripping experiment has been employed as it helps in eliminating the morphological effect of the as-prepared pellet as well as the uncertainties of the bi-directional Li plating-stripping experiment. Using uni-directional Li plating-stripping experiment the critical current density which leads to clear/hard short circuiting of the SE pellet has been stablished. The interface products formed on the Li/SE interface from the Li plating-stripping experiments in the Li|Li symmetric cells are characterised by multinuclear (7Li and 31P) solid-state NMR and X-ray diffraction (XRD) measurements. The chemical stability of the Li8P2S SE with melted Li-metal is also assessed by XRD and (7Li and 31P) NMR measurements. Additionally, the overall (electro-)chemical performance of the fully reduced Li8P2S SE compared to the well-known Li6PS5Br argyrodite SE will be presented.
R.H.C.F. and C.P.G. thank the EU for funding Advanced EU ERC grant (EC H2020 835073). F. N. S. acknowledges funding from The Faraday Institution CATMAT project (FIRG016). S.V. acknowledges funding from the Cambridge Commonwealth European and International Trust, Faraday Institution (SOLBAT, FIRG007), and Royal Society (RP/R1/180147). We acknowledge I11 beamline at the Diamond Light Source, UK, for the synchrotron XRD measurement done under BAG proposal (CY34243).
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