Cerium-doped garnet type LLZO solid electrolyte for inhibiting growth of lithium dendrites and preparation method of cerium-doped garnet type LLZO solid electrolyte

A technology of cerium-doped garnet and solid electrolyte, applied in the manufacture of electrolyte batteries, electrolytes, non-aqueous electrolyte batteries, etc., can solve problems such as lithium dendrite growth, lithium metal negative electrode contact interface impedance, etc., to improve conductivity and reduce Sintering temperature, effect of inhibiting lithium dendrite growth

Pending Publication Date: 2022-05-06
YANGTZE DELTA REGION INST OF UNIV OF ELECTRONICS SCI & TECH OF CHINE HUZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the deficiencies in the prior art, the present invention provides a cerium-doped garnet-type LLZO solid electrolyte that can effectively inhibit the growth of lithium dendrites and a preparation method thereof, so as to solve the problem of lithium dendrites existing in the current garnet-type solid electrolytes. Growth issues and huge interfacial resistance issues in contact with lithium metal anodes

Method used

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  • Cerium-doped garnet type LLZO solid electrolyte for inhibiting growth of lithium dendrites and preparation method of cerium-doped garnet type LLZO solid electrolyte
  • Cerium-doped garnet type LLZO solid electrolyte for inhibiting growth of lithium dendrites and preparation method of cerium-doped garnet type LLZO solid electrolyte
  • Cerium-doped garnet type LLZO solid electrolyte for inhibiting growth of lithium dendrites and preparation method of cerium-doped garnet type LLZO solid electrolyte

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Step 1: batching; LiOH, La2O3, ZrO2, Ta2O5 and CeO2 are weighed according to the chemical formula Li6.8La3Zr1.7Ta0.2Ce0.1O12, wherein in order to avoid volatilization of the lithium source, LiOH is weighed in excess of 10wt%;

[0051] Step 2: One-time ball milling; adopt wet ball milling process, use yttrium stabilized zirconia balls as the ball milling medium, use isopropanol as the ball milling solvent, and carry out according to the mass ratio of mixture: balls: isopropanol is 1:5:1 Grind for 8 hours to obtain a uniformly mixed ball mill;

[0052] Step 3: drying and sieving; drying the ball mill material obtained in step 2 and passing through a 100-mesh sieve to obtain a dry powder;

[0053] Step 4: pre-calcining; the dry powder obtained in step 3 is placed in a magnesia crucible, and pre-fired at 800°C for 10 hours to obtain a pre-fired powder;

[0054] Step 5: Secondary ball milling; the calcined powder obtained in step 4 is subjected to a second ball milling, wit...

Embodiment 2

[0059] Step 1: batching; LiOH, La2O3, ZrO2, Ta2O5 and CeO2 are weighed according to the chemical formula Li6.6La3Zr1.5Ta0.4Ce0.1O12, wherein in order to avoid volatilization of the lithium source, LiOH is weighed in excess of 10wt%;

[0060] Step 2: One-time ball milling; adopt wet ball milling process, use yttrium stabilized zirconia balls as the ball milling medium, use isopropanol as the ball milling solvent, and carry out according to the mass ratio of mixture: balls: isopropanol is 1:5:1 Grind for 6 hours to obtain a uniformly mixed ball mill;

[0061] Step 3: drying and sieving; drying the ball mill material obtained in step 2 and passing through a 100-mesh sieve to obtain a dry powder;

[0062] Step 4: pre-calcining; the dry powder obtained in step 3 is placed in a magnesia crucible, and pre-calcined at 850°C for 8 hours to obtain a pre-calcined powder;

[0063] Step 5: Secondary ball milling; the calcined powder obtained in step 4 is subjected to a second ball milling...

Embodiment 3

[0068] Step 1: batching; LiOH, La2O3, ZrO2, Ta2O5 and CeO2 are weighed according to the chemical formula Li6.4La3Zr1.3Ta0.6Ce0.1O12, wherein in order to avoid volatilization of the lithium source, LiOH is weighed in excess of 10wt%;

[0069] Step 2: One-time ball milling; adopt wet ball milling process, use yttrium stabilized zirconia balls as the ball milling medium, use isopropanol as the ball milling solvent, and carry out according to the mass ratio of mixture: balls: isopropanol is 1:5:1 Grind for 8 hours to obtain a uniformly mixed ball mill;

[0070] Step 3: drying and sieving; drying the ball mill material obtained in step 2 and passing through a 100-mesh sieve to obtain a dry powder;

[0071] Step 4: pre-calcining; the dry powder obtained in step 3 is placed in a magnesia crucible, and pre-calcined at 900°C for 6 hours to obtain a pre-calcined powder;

[0072] Step 5: Secondary ball milling; the calcined powder obtained in step 4 is subjected to a second ball milling...

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Abstract

The invention provides a cerium-doped garnet type LLZO solid electrolyte capable of effectively inhibiting growth of lithium dendrites, the chemical general formula of the cerium-doped garnet type LLZO solid electrolyte is Li < 7-x > La < 3 > Zr < 2-x-y > Ta < x > Ce < y > O < 12 >, x is less than or equal to 0.6, 0lt; y is less than or equal to 0.4 and is of a cubic phase structure with high conductivity. The invention further provides a preparation method of the cerium-doped garnet type LLZO solid electrolyte capable of effectively inhibiting growth of lithium dendrites. The preparation method comprises the steps of material preparation, primary ball milling, primary drying, sieving, pre-sintering, secondary ball milling, secondary drying, sieving, mold pressing, forming, sintering and the like. Under the precondition that a good growth environment is provided for crystal grains through solid-phase sintering, the content of each ion is controlled by comprehensively regulating and controlling the values of x and y, so that the purpose of comprehensively regulating and controlling the performance of the garnet type solid electrolyte material is achieved, and the prepared solid electrolyte material is highly compact in microstructure, free of pores and micro-cracks and high in stability. The material has a typical high-conductivity cubic phase structure, has higher conductivity and lower sintering temperature, and can more effectively inhibit the growth of lithium dendrites.

Description

technical field [0001] The invention relates to the technical field of preparation of all-solid-state electrolyte materials, in particular to a cerium-doped garnet-type LLZO solid-state electrolyte that effectively inhibits the growth of lithium dendrites and a preparation method thereof. Background technique [0002] Solid-state batteries have the advantages of high energy density, wide temperature range, and fewer safety hazards, and are considered to be a promising energy storage technology that can replace lithium-ion batteries based on organic liquid electrolytes. As the most critical component of solid-state batteries, solid-state electrolytes will largely lead the development of future batteries. Among different types of solid-state electrolytes, garnet-type Li 7 La 3 Zr 2 o 12 (abbreviated as LLZO) solid-state electrolyte has a particularly high ionic conductivity (10 -4 to 10 -3 S / cm) and good chemical stability to lithium metal, it is a solid-state lithium me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/058H01M10/0525
CPCH01M10/0562H01M10/058H01M10/0525H01M2300/002Y02P70/50Y02E60/10
Inventor 徐自强胡鑫方梓烜吴孟强
Owner YANGTZE DELTA REGION INST OF UNIV OF ELECTRONICS SCI & TECH OF CHINE HUZHOU
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