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Preparation and surface treatment method of garnet-type solid electrolyte material of solid lithium battery and application

A solid electrolyte, garnet-type technology, applied in the manufacture of electrolyte batteries, electrolytes, non-aqueous electrolyte batteries, etc., can solve problems such as volume energy density limitation of practical applications

Pending Publication Date: 2019-11-26
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these studies have greatly improved the interface between Li metal and garnet, their practical applications are still limited by strict experimental conditions or by sacrificing part of the volumetric energy density.

Method used

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  • Preparation and surface treatment method of garnet-type solid electrolyte material of solid lithium battery and application
  • Preparation and surface treatment method of garnet-type solid electrolyte material of solid lithium battery and application
  • Preparation and surface treatment method of garnet-type solid electrolyte material of solid lithium battery and application

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Effect test

Embodiment 1

[0044] A lithium-lithium symmetric battery based on a surface-treated garnet-type solid electrolyte, including LLZO treated by ALD. First, LLZO is prepared. The material is synthesized by a solid-phase method. The steps are: using lithium hydroxide monohydrate, oxidation Lanthanum, zirconium dioxide, niobium pentoxide, and calcium carbonate were used as metal sources for preparing LLZO.

[0045] First, pre-burn lithium hydroxide monohydrate at 200°C for 6 h (in air); pre-burn lanthanum oxide at 900°C for 12 h (in air), and then according to the stoichiometric ratio (7 : 2.75 : 0.25 : 1.75 : Molar ratio of 0.25) Weigh 50 grams of lithium hydroxide monohydrate, lanthanum oxide, calcium carbonate, zirconium dioxide, and niobium pentoxide after pre-calcination, mix them and ball mill them at a speed of 1400 r / min for 30 min ( SFM-3 high-speed three-dimensional pendulum vibration ball mill, Hefei Kejing Technology Co., Ltd.), calcined at 900 ° C (in air) for 6 h in a muffle furnace...

Embodiment 2

[0054] Lithium hydroxide monohydrate, lanthanum oxide, zirconium dioxide, niobium pentoxide, and calcium carbonate were used as metal sources for preparing LLZO. First, pre-burn lithium hydroxide monohydrate at 200°C for 6 h (in air); pre-burn lanthanum oxide at 900°C for 12 h (in air), and then according to the stoichiometric ratio (7 : 2.75 : 0.25 : 1.75 : Molar ratio of 0.25) Weigh 50 grams of pre-calcined lithium hydroxide monohydrate, lanthanum oxide, calcium carbonate, zirconium dioxide, and niobium pentoxide, mix and ball mill them for 30 minutes, and use a muffle furnace at 900°C Calcined in air for 6 h, after cooling, wet ball milling with 150 ml of isopropanol, and ball milling with a planetary ball mill for 12 h to obtain cubic phase LLZO powder, and finally tableted with a pressure of 25 MPa and sintered at 1100 After sintering at ℃ (in air) for 6 h, a solid electrolyte (LLZO) was obtained. After sintering at 1100 ℃, the bulk density was lower than that at 1200 ℃, ...

Embodiment 3

[0056]A lithium-lithium symmetrical battery based on a garnet-type solid electrolyte, including a garnet-type solid electrolyte, the material is prepared by a solid-phase synthesis method, and the steps are: using lithium hydroxide monohydrate, lanthanum oxide, zirconium dioxide, Niobium and calcium carbonate were used as metal sources for preparing LLZO. First, pre-burn lithium hydroxide monohydrate at 200°C for 6 h (in air); pre-burn lanthanum oxide at 900°C for 12 h (in air), and then according to the stoichiometric ratio (7 : 2.75 : 0.25 : 1.75 : Molar ratio of 0.25) Weigh 50 grams of pre-calcined lithium hydroxide monohydrate, lanthanum oxide, calcium carbonate, zirconium dioxide, and niobium pentoxide, mix and ball mill them for 30 minutes, and use a muffle furnace at 900°C Calcined in air for 6 h, after cooling, wet ball milled with 150 ml of isopropanol, and ball milled with a planetary ball mill for 12 h to obtain cubic phase LLZO powder, and finally tableted with a p...

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Abstract

The invention relates to a preparation and surface treatment method of garnet-type solid electrolyte material of a solid lithium battery and application. The same is a method of preparation of a garnet-type solid electrolyte and interface treatment of low impedance between the same and a lithium anode, a solid-phase synthesis method is used to prepare the garnet-type solid electrolyte, SnO <2> (with thickness of 12.3 mm or the like) is deposited on a surface of the solid electrolyte through atomic layer deposition (ALD) technology, a current buffer layer increases contact tightness between thesolid electrolyte and the lithium anode, and the interface impedance is reduced from 1009.7 Omega to 42.7 Omega. LLZO after ALD treatment is used as a lithium-lithium symmetrical battery of the solidelectrolyte, growth of lithium dendrites is effectively suppressed in constant-current charging and discharging processes, and the same has stable electrochemical behaviors. The treatment method hasthe advantages of cheapness, easy obtaining, high efficiency and convenience.

Description

technical field [0001] The present invention relates to a preparation, surface treatment method and application of a garnet-type solid electrolyte material for a solid-state lithium battery, in particular to the preparation of a garnet-type solid electrolyte and the treatment method for the interface between the solid electrolyte and a lithium negative electrode, and includes passing through the interface Processed Li-Li symmetric batteries with solid-state electrolytes. Background technique [0002] Garnet-type solid electrolyte Li 7 La 3 Zr 2 o 12 Due to its high ionic conductivity, wide electrochemical window and good chemical and electrochemical stability, the application of lithium negative electrodes is possible, and it is considered to be one of the ideal solid-state electrolytes for all-solid-state batteries. However, the development of all-solid-state batteries based on garnet-type solid-state electrolytes still faces many problems, such as the volume change of ...

Claims

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Application Information

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IPC IPC(8): H01M10/0562H01M10/058H01M10/0525
CPCH01M10/0562H01M10/058H01M10/0525H01M2300/0071Y02E60/10Y02P70/50
Inventor 周震唐宾高龙雪刘俊庆
Owner NANKAI UNIV
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