Solid electrolyte, composite integrated positive electrode, integrated battery and preparation method thereof

A technology of solid electrolyte and electrolyte membrane, which is applied in the field of integrated battery and its preparation, composite integrated positive electrode, and solid electrolyte, which can solve the problems of unstable CNT attachment and easy drop, achieve excellent stability, improve conductivity, and purity high effect

Active Publication Date: 2021-01-08
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation method of the composite integrated positive electrode has the disadvantage that CNTs are not stable and easy to fall off on the nickel foam.

Method used

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  • Solid electrolyte, composite integrated positive electrode, integrated battery and preparation method thereof
  • Solid electrolyte, composite integrated positive electrode, integrated battery and preparation method thereof
  • Solid electrolyte, composite integrated positive electrode, integrated battery and preparation method thereof

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preparation example Construction

[0039]The present invention provides a method for preparing a solid electrolyte, which adopts a two-step method of high-temperature solid-phase pre-firing-firing, and includes the following steps:

[0040]S1: Disperse powdered lithium hydroxide, lanthanum trioxide, zirconium dioxide and tantalum pentoxide in isopropanol according to a predetermined ratio, and ball mill for 8-12h at 300-400rpm to obtain slurry ; Then, the ground slurry is vacuum dried at 70-90° C. for 10-15h to obtain a mixed powder;

[0041]S2, pre-fired the mixed powder prepared in step S1 at 940-960°C for 4-8 hours to obtain a pre-fired powder, and then subject the pre-fired powder to grinding treatment;

[0042]S3, the pre-fired powder after the grinding treatment in step S2 is fired at 1050 to 1150°C for 12 to 16 hours to obtain the solid electrolyte.

[0043]As a further improvement of the present invention, the mass ratio of lithium hydroxide, lanthanum trioxide, zirconium dioxide and tantalum pentoxide is (0.36 to 0.43):...

Embodiment 1

[0053]1. Solid electrolyte Li6.7La3Zr1.7Ta0.3O12(LLZTO) Synthesis:

[0054]It is prepared by a two-step method of high-temperature solid phase pre-firing-firing, including the following steps:

[0055]S1, according to the mass ratio of 0.36:1:0.43:0.14, put powdered lithium hydroxide, lanthanum trioxide, zirconium dioxide and tantalum pentoxide into the agate ball mill tank, and use isopropanol as the dispersion liquid. Ball milling at a speed of 350 rpm for 10 hours to obtain a slurry; then, putting the milled slurry in a vacuum oven at 80° C. for vacuum drying for 12 hours to obtain a mixed powder;

[0056]S2, placing the mixed powder prepared in step S1 in a corundum crucible, pre-fired at 950°C for 6 hours (air atmosphere) to obtain a pre-fired powder, and then subject the pre-fired powder to grinding treatment;

[0057]S3, the pre-fired powder after the grinding treatment in step S2 is fired at 1100° C. for 14 hours to obtain LLZTO powder, which is the solid electrolyte.

[0058]2. Preparatio...

Embodiment 2-3

[0091]The difference from embodiment 1 is that in the LLZTO / PVDF composite polymer electrolyte membrane, the mass ratio of LLZTO and PVDF is different, and the other steps are the same as those in uniform embodiment 1, and will not be repeated here.

[0092]Table 2 shows the process parameter settings and performance parameters in Examples 1-3

[0093] Example Mass ratio of LLZTO and PVDF Conductivity Example 1 12：5.146.4×10 -4 S·cm -1

[0094]It can be seen from Table 2 that the influence of the mass ratio of LLZTO and PVDF on the conductivity of the composite polymer electrolyte membrane is: the higher the relative content of LLZTO, the higher the conductivity, but when it increases to a certain value (the mass ratio of LLZTO and PVDF is about 12: 5.14), the conductivity increase is not obvious.

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Abstract

The invention provides a solid electrolyte, a composite integrated positive electrode, an integrated battery and a preparation method thereof. According to the invention, the high-conductivity solid electrolyte is prepared and synthesized by adopting a two-step method of high-temperature solid-phase pre-firing and then firing, and the composite polymer electrolyte membrane is prepared by adoptinga simple solution pouring method. And then, through physical stacking and simple rolling treatment of the composite polymer electrolyte membrane and a positive electrode material, the composite integrated positive electrode with excellent electrochemical performance can be prepared. The integrated battery assembled by the composite integrated positive electrode can effectively improve the contactperformance between the positive electrode and a solid electrolyte, reduces the interface impedance, and has excellent cycle life and coulombic efficiency. The preparation method provided by the invention is simple in process and controllable in process.

Description

Technical field[0001]The invention relates to the technical field of battery preparation, in particular to a solid electrolyte, a composite integrated positive electrode, an integrated battery and a preparation method thereof.Background technique[0002]In recent years, solid-state lithium-ion batteries have the advantages of high safety performance and long cycle life, and have become a research hotspot in the field of new lithium battery technology. However, the current selection of solid electrolyte materials has become a material bottleneck for solid-state lithium-ion batteries towards large-scale commercial applications. Among them, organic-inorganic composite solid electrolyte films have excellent flexibility, interface compatibility, and are suitable for large-scale preparation. The advantages are getting more and more attention from researchers. However, the electrochemical performance of the organic-inorganic composite solid electrolyte film materials currently developed is s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/0525
CPCH01M10/0562H01M10/0525H01M2300/0071Y02E60/10
Inventor 李程张炜鑫曹元成
Owner HUAZHONG UNIV OF SCI & TECH
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