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Erbium-doped cubic phase garnet type solid electrolyte material and synthesis method thereof

A technology of solid electrolyte and synthesis method, applied in circuits, electrical components, secondary batteries, etc., can solve the problems of adverse effects on material morphology and structure, difficult source of raw materials, high sintering temperature, and achieve the overall process flow and short time-consuming, The effect of short grinding time and lower calcination temperature

Inactive Publication Date: 2019-11-12
UNIV OF ELECTRONIC SCI & TECH OF CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Song et al [Shidong S, Butian C, Yanli R, et al. J. Electrochimica Acta, 2018, 270:501-508] used Gd instead of Zr to obtain a stable cubic phase garnet structure with a maximum conductivity of 2.3× 10 -4 S cm -1 , but the sintering temperature is as high as 1220 ° C, and the energy consumption is large; the Chinese patent name is a tantalum-doped cubic garnet structure Li 7 La 3 Zr 2-x Ta x o 12 In the application documents of the material and its preparation method (patent application number: 201510682467.3), the cubic phase garnet structure obtained by replacing Zr with Ta is stable and has good performance. Isopropanol is the ball milling medium, the ball milling speed is 400rpm, after 12 hours of ball milling, it is dried at 70°C for 4 to 6 hours, and then roasted at 900°C for 10 hours." The ball milling time is longer, which has adverse effects on the shape and structure of the material. impact, and the operation is complicated, and the source of raw materials is difficult

Method used

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  • Erbium-doped cubic phase garnet type solid electrolyte material and synthesis method thereof
  • Erbium-doped cubic phase garnet type solid electrolyte material and synthesis method thereof
  • Erbium-doped cubic phase garnet type solid electrolyte material and synthesis method thereof

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Embodiment 1

[0035] This embodiment is matrix phase Li 7 La 3 Zr 2 o 12 The preparation method of this method is taken as an example, compared with Example 2~Example 5.

[0036] Specifically, the steps of the preparation method are as follows: Weigh 1.6423g of lithium acetate [CH 3 COOLi·2H 2 O], 0.9775g lanthanum oxide [La 2 o3 ], 1.84ml zirconium acetate [Zr(CH 3 COO) 4 ], weighing 1.1346g oxalic acid [H 2 C 2 o 4 2H 2 O] Dissolve oxalic acid in 300ml of deionized water, stir and add lanthanum oxide, then add lithium acetate and zirconium acetate in sequence, then stir for 6 hours at a temperature of 120°C and a speed of 600rpm until the remaining 120ml of solution is obtained to obtain 0.2mol / L Metal salt mixed solution; then weigh 3.5482g citric acid [C 6 h 8 o 7 ·H 2 O] added to the metal salt mixed solution, stirred for 3 hours at a temperature of 120 °C and a speed of 600 rpm to obtain a precursor cloudy liquid; the precursor cloudy liquid was dried in a drying oven f...

Embodiment 2

[0039] This embodiment is a doped phase Li 7.05 La 3 Zr 1.95 Er 0.05 o 12 (i.e. x=0.05) preparation method, concrete steps are as follows:

[0040] Specifically, the steps of the preparation method are as follows: Weigh 3.3081g of lithium acetate [CH 3 COOLi·2H 2 O], 1.955g lanthanum oxide [La 2 o 3 ], 2.6460g zirconium nitrate [Zr(NO 3 ) 4 ·5H 2 O], 0.0922g erbium nitrate [ErH 12 N 3 o 15 ], weighing 2.3295g oxalic acid [H 2 C 2 o 4 2H 2 O] Dissolve oxalic acid in 240ml of deionized water, stir and add lanthanum oxide, then add lithium acetate and zirconium acetate in turn, then stir for 5h at a temperature of 110°C and a speed of 500rpm until the remaining 80ml of solution is obtained to obtain 0.6mol / L Metal salt mixed solution; then weigh 7.1218g citric acid [C 6 h 8 o 7 ·H 2 O] Add it to the mixed metal salt solution, stir for 2.5 hours at a temperature of 110°C and a rotation speed of 500rpm to obtain a uniform precursor cloudy liquid; the precursor ...

Embodiment 3

[0043] This embodiment is a doped phase Li 7.1 La 3 Zr 1.9 Er 0.1 o 12 (i.e. x=0.10) preparation method, concrete steps are as follows:

[0044] Specifically, the steps of the preparation method are as follows: Weigh 6.6632g of lithium acetate [CH 3 COOLi·2H 2 O], 3.9100g lanthanum oxide [La 2 o 3 ], 6.98ml zirconium acetate [Zr(CH 3 COO) 4 ], 0.3114g erbium oxalate [Er 2 (C 2 o 4 ) 3 10H 2 O], weighing 4.8250g oxalic acid [H 2 C 2 o 4 2H 2 O] Dissolve oxalic acid in 200ml of deionized water, stir and add lanthanum oxide, then add lithium acetate and zirconium acetate in turn, then stir for 4h at a temperature of 100°C and a speed of 400rpm until the remaining 50ml of solution is obtained to obtain 0.8mol / L Metal salt mixed solution; then weigh 14.2790g citric acid [C 6 h 8 o 7 ·H 2 O] added to the metal salt mixed solution, stirred at a temperature of 100°C and a speed of 400rpm for 2h to obtain the precursor turbid solution; the precursor turbid solutio...

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Abstract

The invention discloses an erbium-doped cubic phase garnet type solid electrolyte material and a synthesis method thereof. The stoichiometric formula of the doped solid electrolyte material is Li7+xLa3Zr2-xErxO12, wherein x is greater than or equal to 0.05 and less than or equal to 0.25. The synthesis method disclosed by the invention comprises the following steps of dissolving a lanthanum sourcecompound in an oxalic acid aqueous solution, sequentially adding a lithium source, a zirconium source and an erbium source compound, heating and stirring uniformly on a magnetic stirrer, then adding citric acid to generate milk white turbid liquid, drying in a drying box for 24 hours, and carrying out pre-sintering, tabletting and calcining to synthesize the solid electrolyte material, wherein thesolid electrolyte synthesized by the method is high in stability at room temperature, relatively high in ionic conductivity and relatively high in application value in the field of solid-state lithium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of solid-state electrolyte materials for lithium-ion solid-state batteries, and in particular relates to an erbium-doped cubic-phase garnet-type solid-state electrolyte material and a synthesis method thereof. Background technique [0002] All-solid-state lithium-ion batteries are considered to be widely used in electronic products, transportation, national defense, aerospace, energy storage and other fields due to their excellent characteristics such as high energy density, high safety, and excellent temperature stability. In recent years, with the rapid development of the electric vehicle industry, the requirements for high energy density and safety of lithium-ion batteries have become higher and higher. [0003] As the core material of all-solid-state lithium-ion batteries, solid electrolyte materials play the role of transporting ions between the positive and negative electrodes. It determines the power...

Claims

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Application Information

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IPC IPC(8): H01M10/0525H01M10/0562
CPCH01M10/0525H01M10/0562Y02E60/10
Inventor 卢伟杨仕清卢超梁桃华
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA