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Boron-doped garnet type LLZO lithium ion conductor and preparation method thereof

A garnet-type, lithium-ion technology, applied in electrochemical generators, electrical components, electrolyte immobilization/gelation, etc., can solve the problems of boron ions not shown, and achieve good electrochemical stability and high ion conductivity rate effect

Active Publication Date: 2016-10-12
SHANGHAI JIAO TONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Kotobuki et al. reported in Ceramics International 40, 5043 (2014) that a sol-gel process was used to prepare undoped cubic phase LLZO, and the ionic conductivity at room temperature was 1.5×10 -4 S / cm, K. Tadanaga et al. reported in Solid State Ionics 285,6 (2016) the preparation of Li by sol-gel process at low temperature 7 La 3 (Zr 2-x Nb x )O 12 (LLZNbO, x=0~1.5), then LiBO 2 and Li 3 BO 3 As a sintering aid, LLZNbO ceramics were sintered at high temperature, and the obtained ionic conductivity was 7×10 -5 S / cm, but this study did not show that boron ions can enter the unit cell of the garnet-type structure

Method used

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  • Boron-doped garnet type LLZO lithium ion conductor and preparation method thereof
  • Boron-doped garnet type LLZO lithium ion conductor and preparation method thereof
  • Boron-doped garnet type LLZO lithium ion conductor and preparation method thereof

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Embodiment 1

[0020] With LiOH, La(NO 3 ) 3 、HBO 2 and ZrO(NO 3 ) 2 As raw material, its molar ratio is LiOH: La(NO 3 ) 3 :HBO 2 :ZrO(NO 3 ) 2 =6.8:2.8:0.2:2.0. Dissolve the raw materials in water to make a solution, then mix according to the above molar ratio, stir and heat to 80°C; put the evenly stirred solution into a microwave reaction vessel; seal the reaction vessel, set the microwave to heat to 250°C for reaction 2 hours; after natural cooling, the solid phase product was separated, washed and dried to obtain the precursor powder. The above precursor powder was formed into a disc with a diameter of 2.0 cm and a thickness of 0.3 cm by cold isostatic pressing at 30 MPa, and then sintered in air at 1180 ° C under normal pressure. After 4 hours of heat preservation, it was naturally cooled to room temperature to obtain a dense ceramic.

[0021]The diameter of the ceramic sample obtained in Example 1 is about 1.8 cm, the thickness is about 0.18 cm, and the gold film is used as ...

Embodiment 2

[0023] Water-soluble LiNO 3 , La(NO 3 ) 3 、H 3 BO 3 and ZrO(NO 3 ) 2 As raw material, its molar ratio is LiNO 3 :La(NO 3 ) 3 :H 3 BO 3 :ZrO(NO 3 ) 2 =7.2:2.4:0.6:2.0. Mix the raw materials according to the above molar ratio, add water, stir and heat to 80°C, stir the solution evenly, and put it into a microwave reaction vessel; seal the reaction vessel, set the microwave to heat to 250°C, and react for 3 hours; after natural cooling, The solid phase product is separated, washed and dried to obtain the precursor powder. The above precursor powder was formed into a disc with a diameter of 2.0 cm and a thickness of 0.3 cm by cold isostatic pressing at 30 MPa, and then sintered in air at 1120 ° C under normal pressure. After 6 hours of heat preservation, it was naturally cooled to room temperature to obtain a dense ceramic.

[0024] The diameter of the ceramic sample obtained in Example 2 is about 1.8 cm, the thickness is about 0.18 cm, and the gold film is used as a...

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Abstract

The invention provides a boron-doped garnet type cubic phase structural LLZO lithium ion conductor. The structural expression formula of the boron-doped garnet type cubic phase structural LLZO lithium ion conductor is Li7La(3-x)BxZr2O12, wherein the x is 0.2 to 0.6. The boron-doped garnet type cubic phase structural LLZO lithium ion conductor has relatively high ionic conductivity and has good electrochemical stability on metallic lithium, can be used as a solid electrolyte of an all-solid-state lithium battery or a lithium ion battery, and can also be used as the solid electrolyte of a metallic lithium-air or metallic lithium-sulphur battery.

Description

technical field [0001] The invention belongs to the field of new energy materials and technologies, in particular to a boron-doped garnet type LLZO ceramic lithium ion conductor. Background technique [0002] Garnet structure Li 7 La 3 Zr 2 o 12 (LLZO) as a solid-state lithium ion conductor was first reported by R. Murugan et al. in Angew. Chem. Int. Ed., 46, 7778 (2007). Due to its good ionic conductivity (>10 -4 S / cm) and the electrochemical stability to metal lithium have received widespread attention, and are ideal electrolyte materials for all-solid-state lithium batteries. However, E. Rangasamya et al. pointed out in Solid State Ionics, 206, 28 (2012) that there are two phase structures in LLZO, namely high-temperature cubic phase and low-temperature tetragonal phase, and their typical ionic conductivities are about 5×10 -4 S / cm and about 1.6×10 -6 S / cm. Obtaining the pure cubic phase of the garnet structure and sintering it into a densified ceramic is the k...

Claims

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Application Information

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IPC IPC(8): H01M10/0562
CPCH01M10/0562H01M2300/0085Y02E60/10
Inventor 孔向阳杨元才叶兵
Owner SHANGHAI JIAO TONG UNIV
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