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Surface modification method of solid electrolyte

A solid electrolyte, surface modification technology, applied in electrolytes, non-aqueous electrolyte batteries, circuits, etc., to achieve the effects of excellent safety and cycle stability, good wettability, and simple process

Pending Publication Date: 2022-03-29
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these modification strategies are relatively strict, and there are still limitations for practical applications, such as the high temperature or corrosive environment required to remove the impurity layer and the expensive equipment required to deposit the lithiophilic layer, etc.

Method used

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  • Surface modification method of solid electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) By traditional solid-state methods, such as high-temperature solid-state reaction, Li 6.5 La 3 Zr 1.5 Ta 0.5 o 12 (LLZTO) synthesized and sintered into ceramic sheets. The final ceramic sheet is about 1.0mm thick and about 13.5mm in diameter;

[0062] (2) Prepare 1M lead acetate aqueous solution, add dropwise 60 microliters of the above aqueous solution on the surface of the solid electrolyte obtained in step (1), react for about 1 minute, rinse with ethanol solvent and dry, and then rapidly heat-treat at 300 degrees for 2 minutes to obtain the final surface modification solid electrolyte;

[0063] (3) Perform the treatment in step (2) on both sides of the solid electrolyte, attach lithium sheets to both sides, and the melting of the fresh Li foil can be continued at a temperature of 200°C to 400°C (for example, 250°C to 350°C) for 1 second to 20 minutes (such as 3 minutes to 10 minutes), then naturally cool to room temperature, and then assemble the button ba...

Embodiment 2

[0071] Step (1) is the same as step (1) in Example 1;

[0072] (2) Prepare a 0.5M zinc nitrate aqueous solution, drop 100 microliters of the above aqueous solution on the surface of the solid electrolyte obtained in step (1), react for about 1.5 minutes, rinse and dry with isopropanol solvent, and then rapidly heat-treat at 300 degrees for 3 minutes Obtain the final surface-modified solid electrolyte;

[0073] Steps (3) and (4) are the same as those in Example 1 (3) and (4);

[0074] Step (5) is the same as step (5) in Example 1, the only difference is that the positive electrode material is LiFePO 4 (LFP) positive electrode;

[0075] (6) Use the LFP positive electrode obtained in the above step (5) to assemble a quasi-solid-state battery. Add an appropriate amount (such as 20 microliters) of electrolyte to the interface of the positive electrode to match the solid electrolyte in step (4), and then assemble the button battery. That is, a quasi-solid lithium metal battery is...

Embodiment 3

[0080] Step (1) is the same as step (1) in Example 1;

[0081] (2) Prepare a 0.8M cobalt nitrate aqueous solution, drop 80 microliters of the above aqueous solution on the surface of the solid electrolyte obtained in step (1), react for about 2 minutes, rinse with ethanol solvent and dry, and then rapidly heat-treat at 400 degrees for 2.5 minutes to obtain the final solution. surface-modified solid electrolytes;

[0082] Step (3) is the same as step (3) in Example 1 to obtain an all-solid lithium symmetric battery.

[0083] The surface-modified electrolyte in the obtained embodiment 3 is subjected to microscopic scanning characterization and surface material characterization, such as Figure 13 , 14 As shown, the surface layer of the electrolyte is uniformly and densely covered with nano-scale particles, and the layer is about 200 nanometers thick, and it is closely and continuously combined with the solid electrolyte. Figure 15 It shows that the electrolyte phase of the a...

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Abstract

The invention relates to a surface modification method of a solid electrolyte, which comprises the following steps: (1) dropwise adding a metal salt aqueous solution on the surface of the solid electrolyte, reacting for 0.1-10 minutes, washing the surface of the solid electrolyte by using a non-aqueous solvent, and drying, the metal salt is at least one of nitrate, acetate, phosphate, chloride and sulfate of metal elements Zn, Al, Pb, Co, Ni, Ag, Fe, Mg, Ti, V, Cr, Mn, Cu, Ga, Ge, Nb, Mo, Sn, In, Sb, W, Ca, Sc, Sr and Ba; and (2) carrying out heat treatment on the dried solid electrolyte at 50-1500 DEG C to obtain the metal oxide surface layer modified solid electrolyte.

Description

technical field [0001] The invention relates to a surface modification method of a solid electrolyte and a solid lithium metal battery containing the solid electrolyte of a modification layer. Background technique [0002] All-solid-state lithium metal batteries are considered to be promising next-generation battery systems. Replacing the flammable organic electrolyte with a solid electrolyte can ensure the high safety of the battery, and the solid electrolyte has strong mechanical properties, which is conducive to inhibiting dendrite growth, and can be matched with an ultra-high-capacity metal lithium anode to increase the energy density of the battery. [0003] However, conventional solid-state Li metal batteries are usually limited by high interfacial resistance between electrodes and solid electrolytes. Due to the rigidity of the ceramic electrolyte and the existence of the impurity layer on the surface, the solid-solid contact between the lithium metal anode and the so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/052
CPCH01M10/0562H01M10/052H01M2300/0071Y02E60/10
Inventor 温兆银蔡明俐姚柳郑楚均靳俊
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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