Method for preparing garnet type Li7La3Zr2O12 electrolyte powder with molten-salt method

A technology of garnet type and electrolyte powder, which is applied in the manufacture of electrolyte batteries, non-aqueous electrolyte batteries, circuits, etc., to achieve good effect, simple preparation process and low cost

Active Publication Date: 2015-02-04
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Garnet structure Li 7 La 3 Zr 2 o 12 The preparation method of LiCl-KCl molten salt of electrolyte powder has not been reported yet

Method used

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  • Method for preparing garnet type Li7La3Zr2O12 electrolyte powder with molten-salt method
  • Method for preparing garnet type Li7La3Zr2O12 electrolyte powder with molten-salt method
  • Method for preparing garnet type Li7La3Zr2O12 electrolyte powder with molten-salt method

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Experimental program
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Effect test

Embodiment 1

[0027] Drying medicines before weighing them: Li 2 CO 3 Dry at 200°C for 6 hours, La 2 o 3 Dry at 900°C for 24 hours, weigh Li according to the stoichiometric ratio of Li:La:Zr=7:3:2 2 CO 3 , La 2 o 3 , ZrO 2, in order to compensate for the loss of lithium in the calcination process, lithium carbonate was increased by 10% according to the mass fraction. Weigh KCl and LiCl according to the KCl:LiCl molar ratio of 58:42. According to Li 2 CO 3 , La 2 o 3 , ZrO 2 The mass ratio of mixture to molten salt is 1:4 to prepare mixed powder. The mixed powder was poured into a zirconia ball mill jar, and ball milled on a planetary ball mill for 10 hours. The ball-milled and mixed powder was dried at 100°C for 10 hours, and packed into a ziplock bag. Take an appropriate amount of mixed powder and place it in an alumina crucible, set the temperature of the electric furnace to 1100°C, place the mixed powder in the electric furnace for 8 hours, cool to room temperature natural...

Embodiment 2

[0030] Drying medicines before weighing them: Li 2 CO 3 Dry at 200°C for 6 hours, La 2 o 3 Dry at 900°C for 24 hours, weigh Li according to the stoichiometric ratio of Li:La:Zr=7:3:2 2 CO 3 , La 2 o 3 , ZrO 2 , in order to compensate for the loss of lithium in the calcination process, lithium carbonate was increased by 10% according to the mass fraction. Weigh KCl and LiCl according to the KCl:LiCl molar ratio of 58:42. According to Li 2 CO 3 , La 2 o 3 , ZrO 2 The mass ratio of mixture to molten salt is 1:4 to prepare mixed powder. The mixed powder was poured into a zirconia ball mill jar, and ball milled on a planetary ball mill for 10 hours. The ball-milled and mixed powder was dried at 100°C for 10 hours, and packed into a ziplock bag. Take an appropriate amount of mixed powder and place it in an alumina crucible, set the temperature of the electric furnace to 900°C, place the mixed powder in the electric furnace for 6 hours, cool it to room temperature natu...

Embodiment 3

[0033] Drying medicines before weighing them: Li 2 CO 3 Dry at 200°C for 6 hours, La 2 o 3 Dry at 900°C for 24 hours, weigh Li according to the stoichiometric ratio of Li:La:Zr=7:3:2 2 CO 3 , La 2 o 3 , ZrO 2 , in order to compensate for the loss of lithium in the calcination process, lithium carbonate was increased by 10% according to the mass fraction. Weigh KCl and LiCl according to the KCl:LiCl molar ratio of 58:42. According to Li 2 CO 3 , La 2 o 3 , ZrO 2 The mass ratio of mixture to molten salt is 1:4 to prepare mixed powder. The mixed powder was poured into a zirconia ball mill jar, and ball milled on a planetary ball mill for 10 hours. The ball-milled and mixed powder was dried at 100°C for 10 hours, and packed into a ziplock bag. Take an appropriate amount of mixed powder and place it in an alumina crucible, set the temperature of the electric furnace to 900°C, place the mixed powder in the electric furnace for calcination for 4 hours, cool it to room ...

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Abstract

The invention relates to a method for preparing garnet type Li7La3Zr2O12 electrolyte powder with a molten-salt method. The method comprises the following steps: weighing Li2CO3, La2O3 and ZrO2 and mixing; adding molten salt and uniformly mixing, and carrying out ball milling, wherein the molten salt is a mixture of KCl and LiCl; heating at 700-1500 DEG C for 2-40 hours; and taking out a product and washing off the molten salt with distilled water and ethanol to obtain nano powder. The method is fast and simple, low in cost and suitable for large-scale production. The prepared Li7La3Zr2O12 powder has small grain diameter, is uniformly distributed and has no clustering.

Description

technical field [0001] The present invention relates to garnet structure Li 7 La 3 Zr 2 o 12 The invention discloses a method for preparing electrolyte powder, belonging to the technical field of preparation of electrolyte materials for lithium ion batteries. Background technique [0002] Solid electrolytes have attracted more and more interest due to their excellent properties and have been developed rapidly. Ramaswamy, Thangadurai, Weppner et al. discovered a Li-ion battery inorganic solid electrolyte material Li with a garnet structure 7 La 3 Zr 2 o 12 . This is a new type of inorganic solid electrolyte material with high conductivity of lithium ions, but its ability to conduct electrons is almost negligible. It is stable to lithium negative electrodes (or lithium alloys) and cobalt, nickel, and manganese positive electrode oxides, and its decomposition voltage is higher than 5.5V. These properties play a big role in obtaining batteries with high energy, high po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/058
CPCH01M10/0562H01M10/058Y02E60/10Y02P70/50
Inventor 冯金奎王宏宽张涛
Owner SHANDONG UNIV
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