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Garnet type solid electrolyte capable of effectively inhibiting lithium dendrites and preparation method of garnet type solid electrolyte

A solid electrolyte and garnet-type technology, which is applied in the manufacture of electrolyte batteries, electrolytes, and non-aqueous electrolyte batteries, etc., can solve problems such as the inability to effectively inhibit the growth of lithium dendrites, intensify the propagation of lithium dendrites, and expand cracks, so as to improve internal Defects, reduced electronic conductivity, and growth-inhibiting effects

Pending Publication Date: 2022-03-25
XI AN JIAOTONG UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in follow-up studies, it was found that the garnet solid electrolyte could not effectively inhibit the growth of lithium dendrites during the application process, and the lithium dendrites permeated and spread to the entire solid electrolyte, eventually leading to the occurrence of short circuits.
At present, researchers believe that there are two main reasons for the growth of lithium dendrites in garnet-type solid electrolytes: one is the high electronic conductivity of garnet-type solid electrolytes, and Li + The combination with electrons is the main reason for the formation of lithium dendrites. Electronic conduction inside the electrolyte induces the formation of dendrites, and lithium dendrites can be directly deposited inside the electrolyte, causing short circuits; the second is the pre-existing defects on the surface and body of the electrolyte, such as Cracks are considered to be an important reason for the growth of lithium dendrites, because dendrites are more likely to grow and gather in defects or cracks, and the stress generated can expand cracks and further aggravate the propagation of lithium dendrites

Method used

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  • Garnet type solid electrolyte capable of effectively inhibiting lithium dendrites and preparation method of garnet type solid electrolyte
  • Garnet type solid electrolyte capable of effectively inhibiting lithium dendrites and preparation method of garnet type solid electrolyte
  • Garnet type solid electrolyte capable of effectively inhibiting lithium dendrites and preparation method of garnet type solid electrolyte

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preparation example Construction

[0034] A method for preparing a garnet-type solid electrolyte that effectively suppresses lithium dendrites, the solid electrolyte has low electronic conductivity at room temperature, comprising the following steps:

[0035] (1) According to the chemical formula Li 7 La 3 Zr 1.5 Ta 0.5 o 12 -xM (LLZTO-xM), the powder of lithium source, lanthanum source, zirconium source and tantalum source is ball milled to obtain raw powder; lithium source needs to be added in excess; the excess quality is 10-10% of the lithium source mass calculated according to the chemical formula 15%; preferably, 2.5%≤x≤15%.

[0036] (2) The raw powder is pre-fired at 750-900°C for 8-10 hours to obtain the initial-fired powder; after this step is pre-fired at a low temperature of 750-900°C, the chemical reaction of the raw powder changes from tetragonal phase to cubic phase.

[0037](3) Weigh a certain mass of initially fired powder, and add a low electronic conductivity material M with a mass fracti...

Embodiment 1

[0051] According to Li 7 La 3 Zr 1.5 Ta 0.5 o 12 -xLiNbO 3 (x=5%) stoichiometric ratio weighs 0.15mol La 2 o 3 , 0.7mol LiOH·H 2 O, 0.15mol ZrO 2 and 0.025mol Ta 2 o 5 , in order to compensate for the volatilization of Li element in the crystal structure at high temperature, the raw material (La 2 o 3 , LiOH·H 2 O, ZrO 2 with Ta 2 o 5 ) in LiOH·H 2 The O excess is 10% by mass based on the stoichiometric ratio. The raw materials were mixed and ball milled in an isopropanol ball milling medium at a speed of 450 r / min for 20 hours, and then dried in an oven at 80° C. for 24 hours to obtain a powder. The obtained powder is ground to uniformity with a mortar, and the masterbatch can be obtained after calcining at 900°C for 9 hours. Take a certain mass of mother powder and a mass fraction of 5% LiNbO 3 , put in a mortar, grind evenly, in a mold with a diameter of 15mm, place the mold on the workbench of the tablet machine, apply a pressure of 400MPa and keep the p...

Embodiment 2

[0053] According to Li 7 La 3 Zr 1.5 Ta 0.5 o 12 -10% LiTaO 3 The stoichiometric ratio weighs 0.15mol La 2 o 3 , 0.7molLiOH·H 2 O, 0.15mol ZrO 2 and 0.025mol Ta 2 o 5 , in order to compensate for the volatilization of Li element in the crystal structure at high temperature, the LiOH·H in the raw material 2 The O excess is 15% by mass based on the stoichiometric ratio. The raw materials were mixed and ball milled in an isopropanol ball milling medium at a speed of 400 r / min for 20 h, and then dried in an oven at 80° C. for 24 h to obtain a powder. The obtained powder is ground to uniformity with a mortar, and the masterbatch can be obtained after calcining at 900°C for 8.5h. Take a certain mass of mother powder and mass fraction of 10% LiTaO 3 , put it in a mortar, grind evenly, in a mold with a diameter of 15mm, place the mold on the table of the tablet machine, apply a pressure of 450MPa and hold the pressure for 5min, then demould and take out the complete green...

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Abstract

The invention discloses a garnet type solid electrolyte capable of effectively inhibiting lithium dendrites and a preparation method thereof, and the preparation method comprises the following steps: carrying out ball milling on a lithium source, a lanthanum source, a zirconium source and a tantalum source according to a chemical formula Li7La3Zr1. 5Ta0. 5O12-xM to obtain raw powder; 2.5% < = x < = 25%; pre-sintering the raw powder to obtain primarily-sintered powder; adding a low-electron conductive substance M into the primarily sintered powder, and uniformly grinding to obtain mother powder; pressing the mother powder into a plain blank sheet; and sintering the blank sheet to obtain the garnet type solid electrolyte capable of effectively inhibiting the lithium dendrites. The preparation method adopts a traditional simple solid-phase sintering preparation process, is completed through a two-step sintering method, has the advantages of being simple in process, easy to operate, high in repeatability, low in production cost and the like, and is suitable for practical application and large-scale production.

Description

technical field [0001] The invention belongs to the technical field of preparation of oxide solid electrolytes, and in particular relates to a garnet-type solid electrolyte capable of effectively suppressing lithium dendrites and a preparation method thereof. Background technique [0002] Lithium-ion batteries (LIBs) have been widely used in higher power mobile electronic devices, electric vehicles, and grid-scale energy storage due to their higher energy density and environmental friendliness. However, most current commercial LIBs employ organic liquid electrolytes, which raise concerns about the safety of Li-ion batteries due to their disadvantages such as flammability, mobility, toxicity, and volatility. Therefore, replacing conventional liquid electrolytes with non-flammable and stable solid electrolytes (SEs) is considered to be the best strategy to overcome the safety challenges of Li-ion batteries. In addition, the energy density of the battery can be greatly improve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0562H01M10/058
CPCH01M10/0562H01M10/058H01M4/5825H01M2300/002Y02E60/10Y02P70/50
Inventor 徐友龙马晓宁
Owner XI AN JIAOTONG UNIV
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