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Sulfide solid electrolyte with core-shell structure, preparation method and solid battery

A technology of solid electrolyte and core-shell structure, which is applied in the direction of secondary batteries, circuits, electrical components, etc., can solve the problem of the decline in the basic performance of sulfide solid electrolytes, such as conductivity, to slow down performance decay, improve stability, and improve weakening effects Effect

Active Publication Date: 2019-11-15
ZHEJIANG FUNLITHIUM NEW ENERGY TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, its shortcoming is that as an oxygen source, it interacts with Li during its preparation process. 2 S, P 2 S 5 The existing binary sulfide electrolyte raw materials are mixed with each other in long-term ball milling, and the oxygen source is evenly dispersed in the Li 2 S, P 2 S 5 In the process of heat treatment, while realizing vitrification, S substitution in P-S is realized, which obtains PS 3 o 3- It is uniformly dispersed in the sulfide solid electrolyte material, resulting in a substantial drop in the basic performance of the sulfide solid electrolyte, and when its surface is in contact with the positive electrode material in the charged state or with oxygen in the air, the deterioration of the sulfide solid electrolyte is slowed down , but still needs to be further improved

Method used

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  • Sulfide solid electrolyte with core-shell structure, preparation method and solid battery
  • Sulfide solid electrolyte with core-shell structure, preparation method and solid battery
  • Sulfide solid electrolyte with core-shell structure, preparation method and solid battery

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0078] The sulfide electrolyte Z was prepared as follows,

[0079] S1: Under the protection of argon atmosphere, weigh the lithium source, M source, Q source and X source according to the composition ratio of the general formula,

[0080] Lithium source: LiH, Li 2 S 2 , Li 2 S. Li 2 Se, Li 2 Se 2 One or more compositions in;

[0081] S source: S, H 2 S, P 2 S 5 ,P 4 S 9 ,P 4 S 3 , Se, P 2 Se 5 , Li 2 S 2 , Li 2 S. Li 2 Se, Li 2 Se 2 One or more compositions in;

[0082] P source: P, P 2 S 5 ,P 4 S 9 ,P 4 S 3 One or more compositions in;

[0083] X source is Li 2 X, X is one of Cl, Br, I, F;

[0084] Under the condition that the water content is less than 10ppm, the lithium source, the M source, the Q source and the X source are ground and mixed evenly to obtain a powder raw material;

[0085] S2: After grinding the powder primary material to a uniform particle size, pressure tableting to obtain a flake primary material;

[0086] S3: Put the flak...

Embodiment 1～6

[0117] 10g Li prepared by Comparative Example 1 6 P.S. 5 Cl was placed in an ellipsoidal quartz bottle (100mL), and a filter cap was added to pump the negative pressure until the air pressure was 0.1 atm, and the NO was injected through a syringe. 2 , placed in a rotary electric furnace, heated and kept warm for surface treatment, and a sulfide solid electrolyte with a core-shell structure is obtained after cooling. The specific parameters of the preparation process are shown in Table 1. [Shell layer thickness test] was carried out on Examples 1-6 at the same time.

[0118] [Shell Thickness Test]

[0119] The sulfide solid electrolyte to be tested was subjected to a stripping-element determination test. The peel depth is referenced to Si. The concentration of O element was measured under different stripping depth conditions; the thickness of the shell was taken when the O element concentration was lower than the detection limit. The results are shown in Table 1.

[0120...

Embodiment 6～8

[0158] An all-solid-state lithium battery. The sulfide solid electrolytes obtained in Examples 1 to 6 and Comparative Example 1 are prepared for positive electrode composites, sulfurized solid electrolytes, and negative electrode composites, and are prepared according to [Preparation method of all-solid lithium batteries] The specific parameters of the solid-state lithium battery are shown in Table 3.

[0159] Among them, the positive electrode compound is selected from LiNi corresponding to the sulfide solid electrolyte and the positive electrode active material. 0.6 co 0.2 mn 0.2 o 2 (NCM622) was weighed at a weight ratio of 3:7 and mixed thoroughly in an agate mortar. The negative electrode composite is made by selecting the corresponding sulfide solid electrolyte and graphite as the negative electrode active material at a weight ratio of 1:1, and fully mixing them in an agate mortar.

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Abstract

The invention relates to a sulfide solid electrolyte and discloses a sulfide solid electrolyte with a core-shell structure, a preparation method and a solid battery, so as to solve the problem that the existing O doping improvement method has limited effects on improvements on the stability of the positive electrode by the sulfide solid electrolyte and falling of conductivity is caused. The sulfide solid electrolyte with a core-shell structure in the technical scheme comprises a core-shell particle with a particle size of 0.5 to 10 mum; the core-shell particle comprises a core and a shell coating the core; the core is a sulfide solid electrolyte material; the thickness of the shell is smaller than 100 nm; and according to the shell, the sulfide solid electrolyte material is oxidized by external oxides, part of P-S bonds or all of the P-S bonds are oxidized and replaced as P-O bonds, the high ion conductivity advantage of the sulfide solid electrolyte is ensured, and the electrochemicalstability of the sulfide solid electrolyte for the high-oxidizability positive electrode active material is further improved.

Description

technical field [0001] The invention relates to a sulfide solid electrolyte, in particular to a core-shell structure sulfide solid electrolyte, a preparation method and a solid-state battery. Background technique [0002] Since the 1990s, Japan's Sony Corporation first successfully launched commercial lithium-ion batteries, lithium-ion batteries have been widely used in portable electronic devices such as mobile phones and notebook computers due to their high power density, high voltage, environmental friendliness, and small self-discharge. and electric vehicles. After years of development, the application field of lithium-ion batteries has developed from small digital electronic products to large-scale energy storage products such as electric vehicles and energy storage power stations. And from 2011 to 2017, the compound annual growth rate of the total demand for lithium battery cells in the world's three major application terminals reached 29.2%, and driven by the develop...

Claims

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Application Information

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IPC IPC(8): H01M10/0525H01M10/0562
CPCH01M10/0562H01M10/0525Y02E60/10
Inventor 许晓雄黄晓张秩华
Owner ZHEJIANG FUNLITHIUM NEW ENERGY TECH CO LTD
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