A method for removing impurities on the surface of lithium lanthanum zirconium oxygen electrolyte for solid lithium batteries

Abstract

The invention relates to the field of oxide solid electrolytes, in particular to a method for removing impurities on the surface of a lithium-lanthanum-zirconium-oxygen electrolyte for a solid-state lithium battery. The method involves transferring the lithium-lanthanum-zirconium-oxygen sheet containing impurities into an analysis chamber of an X-ray photoelectron spectrometer , and then in a vacuum environment, carry out gradual heating to remove impurities on the surface of the lithium lanthanum zirconium oxide sheet, and perform in-situ XPS tests on the surface of the lithium lanthanum zirconium oxide sheet during the gradual heating process, and wait for the impurities on the surface of the lithium lanthanum zirconium oxide sheet to be removed Finally, cool the in-situ heating sample stage to room temperature, then transfer it to the glove box connected to the X-ray photoelectron spectrometer, and remove the lithium lanthanum zirconium oxide sheet from the in-situ heating sample stage in the glove box, Obtain pure lithium lanthanum zirconium oxide sheet. The method of the present invention uses vacuum annealing and in-situ XPS testing, and combines the removal of the impurity layer on the surface of the lithium lanthanum zirconium oxide sheet with the monitoring of surface components, thereby realizing high-precision removal of impurities on the surface of the lithium lanthanum zirconium oxide sheet.

Description

technical field [0001] The invention belongs to the field of oxide solid electrolytes, and in particular relates to a method for removing impurities on the surface of a lithium-lanthanum-zirconium-oxygen electrolyte for a solid-state lithium battery. Background technique [0002] Solid-state lithium batteries have attracted much attention due to their high safety, high energy density and other advantages. There are many kinds of solid electrolytes used in them, among which the garnet-type solid electrolyte lithium lanthanum zirconium oxide Li 7 La 3 Zr 2 o 12 (LLZO) has attracted much attention due to its high ionic conductivity and stability towards lithium anodes. [1,2] . But the solid electrolyte is unstable in the air, firstly with H 2 O reacts to generate LiOH, which is further combined with CO 2 The reaction produces Li 2 CO 3 [3] . The reaction process is rapid and unavoidable, and the reaction layer is mainly located on the surface of the sample. In additio...

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Problems solved by technology

However, these methods still have limitations: since the annealing process is carried out in air, the lithium lanthanum zirconium oxygen samples treated by this method still inevitably generate Li 2 CO 3 , and the organic adsorption layer cannot be removed [6,7] ;Physical methods such as polishing may destroy the properties of the sample, and it is difficult to achieve a good removal effect [3] ;Chemical methods such as pickling introduce additional ingredients [8]

At present, there is no relevant method that can completely remove the surface impurities of lithium lanthanum zirconium oxide without causing additional effects, which restricts the research and further utilization of the intrinsic properties of lithium lanthanum zirconium oxide

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