Lithium-lanthanum-zirconium oxide-based solid electrolyte material with stable surface, and preparation method and application thereof
A technology of solid electrolyte, lithium lanthanum zirconium oxide, applied in the manufacture of electrolyte batteries, electrolytes, non-aqueous electrolyte batteries, etc., can solve the problems of reduced ionic conductivity, large solid electrolyte/electrode interface impedance, safety restrictions on lithium-ion batteries, etc. , to achieve the effects of improving chemical stability, improving energy density and cycle stability, and broadening the application range
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[0040] The preparation method of the lithium lanthanum zirconium oxide solid electrolyte material with stable surface comprises:
[0041] (1) Preparation of the lithium lanthanum zirconium oxide solid electrolyte (LLZO);
[0042] The preparation method of lithium lanthanum zirconium oxide solid electrolyte (LLZO) is a sol-gel method, and the preparation steps include: the precursors of lithium Li, lanthanum La, zirconium Zr and doping element M are prepared according to the formula of Li, La, Zr, M The molar ratio is (5+x): 3:x:(2-x) mixing, adding a solvent to dissolve, adding a chelating agent to form a sol-gel, heating and evaporating the solvent to obtain a mixed powder; grinding the mixed powder, first in Sintering at 250-600° C. for 2-48 hours, grinding again, and sintering at 500-1000° C. for 2-48 hours to obtain the lithium lanthanum zirconium oxide solid electrolyte (LLZO).
[0043] Alternatively, the preparation method of the lithium lanthanum zirconium oxide solid ...
Embodiment 1
[0049] (1) The chemical formula is Li prepared by solid-state reaction method 6.4 La 3 Zr 1.4 Ta 0.6 o 12 Lithium lanthanum zirconium oxide solid electrolyte powder, its preparation steps include: according to the molar ratio of Li, La, Zr, Ta is 6.4:3:1.4:0.6, select LiOH, La 2 o 3 , ZrO 2 and Ta 2 o 5 LiOH is used as a raw material with an excess of 5 wt% LiOH, which is ball-milled in alcohol for 24 hours and then dried; then calcined at 900 °C for 10 hours with a heating rate of 4 °C / min, and after the sintering is completed, the powder is crushed and sieved to obtain Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 Powder (LLZTO), which is sieved to obtain LLZTO powder with uniform particle size.
[0050] (2) The LLZTO powder obtained in step (1) is dispersed in a solvent, and the precursor of the cladding layer material, zirconium oxychloride ZrOCl 2 Dissolve in a solvent containing LLZTO powder, add a chelating agent to form a sol-gel, heat and evaporate the solvent to obtain...
Embodiment 2
[0057] Basically the same as embodiment 1, the difference is that the cladding layer material is the Li of NASICON structure 1.3 al 0.3 Ti 1.7 (PO 4 ) 3 (LATP). In Example 2, a surface-stabilized lithium lanthanum zirconium oxide solid electrolyte material (LATP@LLZTO) was prepared, wherein the content of the coating material LATP was 2 wt%.
[0058] Figure 6 The XRD spectrum of the prepared surface-stabilized lithium lanthanum zirconium oxide solid electrolyte material (LATP@LLZTO) was obtained by Figure 6 It can be seen that the surface-stabilized lithium lanthanum zirconium oxide solid electrolyte material (LATP@LLZTO) still maintains a cubic phase with high ionic conductivity.
[0059] Figure 7 The TEM image of the prepared surface-stabilized lithium-lanthanum-zirconium-based solid electrolyte material (LATP@LLZTO) was obtained by Figure 7 It can be seen that LATP is evenly coated on the surface of LLZTO.
[0060] Preparation of lithium-lanthanum-zirconium-bas...
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