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

A solid electrolyte and electrolyte technology, which is applied in the field of solid electrolyte, composite integrated positive electrode, integrated battery and its preparation, can solve the problems of unstable CNT attachment and easy drop, and achieve simple and easy processing methods, excellent stability, The effect of increasing the conductivity

Active Publication Date: 2022-04-12
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 is prepared by a high-temperature solid phase pre-firing-firing two-step method, including 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 to 12 hours at a speed of 300 to 400 rpm to obtain a slurry ; Then, vacuum-dry the ground slurry at 70-90°C for 10-15 hours to obtain a mixed powder;

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

[0042] S3, firing the calcined powder after the grinding treatment in step S2 at 1050-1150° C. for 12-16 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 pent...

Embodiment 1

[0053] 1. Solid electrolyte Li 6.7 La 3 Zr 1.7 Ta 0.3 o 12 Synthesis of (LLZTO):

[0054] It is prepared by high-temperature solid phase pre-firing-firing two-step method, 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 an agate ball mill jar, use isopropanol as the dispersion liquid, At 350 rpm, ball milling for 10 hours to obtain a slurry; then, put the ground slurry in a vacuum oven at 80° C. for 12 hours to obtain a mixed powder;

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

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

[0058] 2. Preparation of LLZTO / PVDF ...

Embodiment 2-3

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

[0092] Table 2 is the process parameter setting and performance parameter in embodiment 1-3

[0093] Example Mass ratio of LLZTO and PVDF Conductivity Example 1 12：5.14 6.4×10 -4 S cm -1

[0094] It can be seen from Table 2 that the effect 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 will be, 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. The invention adopts a high-temperature solid-phase pre-firing-re-firing two-step method to prepare and synthesize a high-conductivity solid electrolyte, and prepares a composite polymer electrolyte membrane through a simple solution pouring method. Then, through the physical stacking of the composite polymer electrolyte membrane and the cathode material and simple rolling treatment, a composite integrated cathode with excellent electrochemical performance can be prepared. The integrated battery assembled with the composite integrated positive electrode can effectively improve the contact performance between the positive electrode and the solid electrolyte, reduce the interfacial impedance, and have excellent cycle life and Coulombic efficiency. The preparation method provided by the invention has simple process and controllable 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 selection of solid electrolyte materials has become a material bottleneck for large-scale commercial applications of solid-state lithium-ion batteries. Among them, organic-inorganic composite solid-state electrolyte films have excellent flexibility, interfacial compatibility, and are suitable for large-scale preparation. advantages, and more and more researchers pay attention to it. However, the electrochemical properties of the currently developed organic-inorganic composite solid electrolyte thin film mater...

Claims

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Application Information

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