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A kind of garnet type composite electrolyte material and its preparation method and application

A composite electrolyte, garnet-type technology, applied in the field of garnet-type composite electrolyte materials and their preparation, can solve the problem that the garnet-type oxide electrolyte material has not been proposed, is not suitable for large-sized ceramic solid electrolyte materials, and the temperature of the sintering equipment cavity Uneven distribution and other problems, to achieve the effect of low equipment requirements, mild conditions, and reduced energy consumption

Active Publication Date: 2021-04-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of ceramic materials requires long-term sintering at a temperature exceeding 1000°C, and the sintering process consumes time and energy; in addition, the preparation process of ceramic materials is complicated, and there are problems such as uneven temperature distribution in the sintering equipment cavity, which is not suitable for Fabrication of large-scale ceramic solid electrolyte materials
[0007] In order to solve the above problems, at present, the main focus is to reduce the sintering temperature of solid electrolyte ceramic materials by means of ion doping, but there is no solution to the problem of how to obtain a garnet-type oxide electrolyte material with a suitable size.

Method used

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  • A kind of garnet type composite electrolyte material and its preparation method and application
  • A kind of garnet type composite electrolyte material and its preparation method and application
  • A kind of garnet type composite electrolyte material and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0039] In a glove box with argon atmosphere, weigh 0.911g Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 and 0.089g LiBH 4 (among them, Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 with LiBH 4 The molar ratio is 1:4) into the ball milling tank in turn, the ball-to-material ratio is 120:1, and the ball milling beads are made of stainless steel; the mixture is ball milled in a planetary ball mill at a speed of 300rpm for 12h, and the obtained ball milling product is stored in an argon atmosphere glove box. It was taken out and recorded as LLZTO-LBH, and the subsequent electrochemical performance test was carried out.

[0040] Such as figure 1 As shown, in the garnet-type composite electrolyte material (LLZTO-LBH) prepared in Example 1, the black and dense garnet-type oxide is covered with a layer of amorphous phase, which improves the compactness of the garnet-type composite electrolyte material. property, reducing the Li + obstacles in the migration process, thereby further improving the Li + ...

Embodiment 2

[0047] In a glove box with argon atmosphere, weigh 0.911g Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 , 0.089g LiBH 4 and 0.053gLiNH 2 (among them, Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 with LiBH 4 、LiNH 2 The molar ratio is 1:4:2) into the ball milling tank in turn, the ball-to-material ratio is 100:1, and the ball milling beads are made of stainless steel; the mixture is ball milled in a planetary ball mill at a speed of 351rpm for 12h, and the obtained ball milling product is heated in an argon atmosphere. Take it out from the glove box, record it as LLZTO-B-N, and conduct subsequent electrochemical performance tests.

[0048] Such as Figure 7 As shown, A is the XRD spectrum of the garnet-type composite electrolyte material (LLZTO-B-N) prepared in Example 2; B is the original garnet-type oxide (Li 6.4 La 3 Zr 1.4 Ta 0.6 o 12 )2's XRD spectrum, as can be seen from the figure, and LiBH 4 The composite material LLZTO-B-N obtained by ball milling has no new crystal phase format...

Embodiment 3

[0051] In the glove box of argon atmosphere, weigh 0.928g Li 6.4 Al 0.2 La 3 Zr 2 o 12 , 0.072g LiBH 4 (among them, Li 6.4 Al 0.2 La 3 Zr 2 o 12 with LiBH 4 The molar ratio is 1:3) and put into the ball milling tank in turn, the ball-to-material ratio is 90:1, and the ball milling beads are made of stainless steel; the mixture is ball milled in a planetary ball mill at a speed of 290rpm for 20h, and the obtained ball milling product is placed in an argon atmosphere glove Take it out of the box, record it as LALZO-LBH, and conduct subsequent electrochemical performance tests.

[0052] Such as Figure 9 Shown, the impedance (EIS) curve of embodiment 3 garnet type composite electrolyte material (LALZO-LBH), the curve is a semicircle in the high-frequency region, and the intersection point of the right end of the semicircle and the real axis represents the total resistance of the bulk phase and the particle gap. The low frequency region is a slanted line, which reflect...

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Abstract

The invention discloses a garnet-type composite electrolyte material and a preparation method thereof, belonging to the field of new energy materials. The garnet-type composite electrolyte material is a core with a garnet-type oxide as the core and a coordination hydride as the shell shell structure; the preparation method of the garnet-type composite electrolyte material of the present invention, comprising: under the protection of an inert gas, redox reactions occur between the garnet-type oxide and the coordination hydride under the action of ball milling to obtain the garnet-type composite electrolyte material electrolyte material. The garnet-type composite electrolyte material prepared by the present invention has the advantages of high lithium ion conductivity and high voltage window, can be applied to the preparation of all-solid lithium-ion batteries, and has high application value in the industrial production of all-solid-state lithium-ion batteries .

Description

technical field [0001] The invention relates to the field of new energy materials, in particular to a garnet-type composite electrolyte material and a preparation method thereof. Background technique [0002] All-solid-state lithium-ion batteries have the advantages of high energy density, non-spontaneous combustion, and no pollution, and are compatible with high-capacity metallic lithium negative electrodes and high-voltage positive electrodes, and have a wide range of applications in real life. Among them, the electrolyte material, as one of the important components of the all-solid-state lithium-ion battery, has a great influence on the performance of the battery; and the garnet-type oxide electrolyte material has the advantages of high ion conductivity, environmental friendliness and high safety performance. A class of all-solid-state lithium-ion battery electrolyte materials with development potential. [0003] For cubic garnet-type oxides Li 7 La 3 Zr 2 o 12 , who...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562H01M10/0525H01M10/058
CPCH01M10/0525H01M10/0562H01M10/058H01M2300/0071H01M2300/0094Y02E60/10Y02P70/50
Inventor 刘永锋高源潘洪革高明霞
Owner ZHEJIANG UNIV
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