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A kind of Ga, Al co-doped llzo solid electrolyte, multi-element solid battery and preparation method thereof

A solid-state battery, solid electrolyte technology, used in electrolytes, electrical components, secondary batteries, etc., can solve the problems of high electrolyte strength and brittleness, irregular deposition of lithium ions, and inability to operate solid batteries, to ensure normal performance and reliability. Cycling, preventing the formation of lithium dendrites, and slowing down the decay of discharge capacity

Active Publication Date: 2021-10-19
GUANG DONG DONGBOND TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Different from the electrolyte, the LLZO electrolyte has high strength and high brittleness, and it is difficult to fully contact with the positive and negative materials, and this insufficient solid-solid contact will lead to a huge interface impedance between the electrolyte and the electrode, and a poor negative / electrode The impedance of the electrolyte interface is about 1KΩ·cm2, and the impedance of the positive electrode / electrolyte interface without modification is often higher than 1MΩ·cm2. Such a high interface impedance makes solid batteries unable to operate at room temperature, so the interface problem is that LLZO is used Top hurdles to practical application in solid-state batteries
[0005] In addition to the interface problem, another major problem of LLZO electrolytes in battery applications is the growth of lithium dendrites. It was first believed that the strength of inorganic solid electrolytes is high, and lithium dendrites cannot pierce them, so there is no problem of lithium dendrites. However, research It is shown that the position of lithium ions passing through the LLZO electrolyte ion channel reaches the negative electrode is uneven, and there is also a gap between the solid electrolyte and the negative electrode interface, so it is easy to cause irregular deposition of lithium ions, thereby forming lithium dendrites, and once lithium dendrites Appearance means that the lithium ions inside the battery have irreversibly decreased, and at the same time, lithium dendrites will continue to absorb free lithium ions to grow, and eventually may puncture the diaphragm, resulting in direct contact between the positive and negative electrodes of the battery and causing a short circuit

Method used

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  • A kind of Ga, Al co-doped llzo solid electrolyte, multi-element solid battery and preparation method thereof
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  • A kind of Ga, Al co-doped llzo solid electrolyte, multi-element solid battery and preparation method thereof

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Experimental program
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Embodiment 1

[0053] Embodiment 1 (preparation of Ga, Al co-doped LLZO solid electrolyte)

[0054] According to the chemical formula Li 7-3x-3y al x Ga y La 3 Zr 2 o 12 , (wherein x=0.15, y=0.15) molar ratio weighs lithium hydroxide monohydrate (LiOH·H 2 O), lanthanum trioxide (La 2 o 3 ), zirconium dioxide (ZrO 2 ), gallium trioxide (Ga 2 o 3 ), aluminum oxide (Al 2 o 3 ), the La 2 o 3 Sinter in a muffle furnace at 900°C for 12 hours. After sintering, mix it with lithium hydroxide monohydrate, zirconium dioxide, gallium trioxide, and aluminum trioxide. The raw materials are wet ball milled for 10 hours (the balls and jars are both made of zirconia) to ensure that the raw materials are mixed evenly; the raw materials mixed by ball milling are dried in a vacuum oven at 80°C for 12 hours; the dried and evenly mixed raw materials are ground Thinning, pre-sintering at 950°C for 6 hours to obtain the precursor material; weigh a certain mass of the precursor material obtained by pr...

Embodiment 2

[0055] Embodiment 2 (preparation of positive electrode sheet)

[0056] The starch was dried at 100°C for 24 hours in an air atmosphere, and then the dried starch was ball milled at a speed of 300r / min, and the ball milling time was 6 hours. Finally, the ball milled starch was put into a quartz tube furnace. Under the protection of nitrogen atmosphere, at a heating rate of 10°C / min, the first step is to 200°C, and the temperature is kept at 200°C for 1 hour, and then the temperature is kept at 500°C for 1 hour, and the positive electrode active material is obtained in the natural cooling zone to room temperature. . Coating the cathode active material slurry on the quantum carbon-based film coated with a layer of nano-silver metal protection to obtain two coating materials, and then hot-compressing the two coating materials to form a quantum carbon-based film / metal protection Layer / positive electrode material / metal protective layer / quantum carbon-based film multilayer composite...

Embodiment 3

[0057] Embodiment 3 (preparation of multi-component negative pole sheet)

[0058] Below -50°C, under vacuum conditions, 90% by weight of metal lithium is placed in a molten alloy bath, and then gold lithium is heated to 300°C to melt metal lithium; then according to the weight ratio of 5% nickel, Add 3% manganese into the molten bath and stir for 30 minutes; then add 2% gallium into the molten bath and keep stirring for 30 minutes to completely dissolve the gallium particles and homogenize the liquid mixture to form a molten alloy, then cool to room temperature, A gallium-doped lithium-nickel-manganese multi-element active material is prepared.

[0059] Coat the negative electrode active material slurry on the quantum carbon-based film coated with a layer of nano-silver metal protection to obtain two coating materials, and then heat-compress the two coating materials to form a quantum carbon-based film / metal Multi-layer composite multi-element negative electrode sheet of prot...

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Abstract

The invention belongs to the technical field of all-solid-state batteries, and in particular relates to a Ga, Al co-doped LLZO solid electrolyte, a multi-component solid-state battery and a preparation method thereof. The Ga, Al co-doped LLZO inorganic oxide solid electrolyte prepared by the invention has ion conductivity High efficiency, good stability and other excellent performance. The invention introduces Ga, Al co-doped LLZO inorganic oxide solid electrolyte and quantum carbon-based film / metal composite interface layer to prepare multi-component solid-state battery, which effectively solves the three major problems of lithium dendrite growth, low Coulomb effect and interface side reaction. The core problem faced by the mass production of solid-state batteries.

Description

technical field [0001] The invention relates to a Ga and Al co-doped LLZO solid electrolyte, a multi-component solid-state battery and a preparation method thereof, belonging to the technical field of solid-state batteries. Background technique [0002] Inorganic oxide solid electrolyte has the advantages of high thermal stability, chemical stability, good ion conductivity, large potential window, relatively high calcination density, no environmental pollution, and controllable process conditions, and has gradually become a new An important material for a generation of all-solid power batteries. Among them, the garnet-type solid electrolyte (LLZO) is the electrolyte with the best comprehensive performance among the oxide electrolytes. The LLZO solid electrolyte not only has a conductivity as high as 10-4S / cm~10-3S / cm, but also has chemical stability to Li And the shear modulus of 56GPa ~ 60GPa, it may become the core material of the next generation of batteries - all solid-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/0562
CPCH01M10/0562H01M2300/0071H01M2300/0077Y02E60/10
Inventor 刘萍
Owner GUANG DONG DONGBOND TECH CO LTD
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