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Organic/inorganic composite solid electrolyte and preparation method thereof

A solid electrolyte and inorganic composite technology, which is applied in the direction of circuits, electrical components, secondary batteries, etc., can solve the problems of affecting the electrochemical cycle performance of solid-state batteries, reducing the crystallinity of organic polymers, and increasing interface resistance, so as to avoid heat treatment The effect of high temperature, inhibition of interface reaction, and reduction of interface resistance

Active Publication Date: 2019-06-14
深圳索理德新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the interface between the sulfide solid electrolyte and the metal lithium negative electrode will react, causing the sulfur-based solid electrolyte to decompose, increasing the interface resistance between the electrolyte and metal lithium, and affecting the electrochemical cycle performance of the solid-state battery.
Organic solid electrolytes have good film-forming properties and flexibility, but have low ionic conductivity at room temperature
For example, the patent No. CN105680092 A proposes to add a certain amount of silicon dioxide to reduce the crystallinity of organic polymers, thereby improving the ionic conductivity of organic solid electrolytes. The ionic conductivity of ~10 was obtained by testing at 60°C. -4 S / cm, relative to the current commercial application at room temperature ~ 10 -2 The ionic conductivity of S / cm is much lower
The preparation of sulfides by the liquid phase method has the characteristics of simple operation and controllability, but the organic / inorganic composite solid electrolyte formed in situ in the liquid phase has certain limitations.

Method used

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  • Organic/inorganic composite solid electrolyte and preparation method thereof
  • Organic/inorganic composite solid electrolyte and preparation method thereof
  • Organic/inorganic composite solid electrolyte and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Lithium sulfide and phosphorus pentasulfide were ground and mixed in a mortar at a ratio of 1:1 (molar ratio), ball milled in a ball mill for 6 hours, and heat treated at 280°C for 4 hours to obtain a sulfur-based solid electrolyte. PMMA polymer and LiClO 4 Mix at a molar ratio of 10:1, add the sulfide powder and polymer / lithium salt into n-heptane at a mass ratio of 9:1, stir magnetically at 50°C for 12 hours, remove the organic solvent by rotary evaporation, and dry at 80°C , to obtain an organic / inorganic composite solid electrolyte. The thickness of the coating layer of the organic polymer is 20-30nm, and the ion conductivity at room temperature is 10 -4 S / cm.

[0052] On the one hand, the preparation method is suitable for preparing three-phase and above sulfur-based solid electrolytes, and is also suitable for organic polymer electrolytes with low decomposition temperatures. In addition, the composite electrolyte uses an organic solid electrolyte to coat the sul...

Embodiment 2

[0055] Lithium sulfide, phosphorus pentasulfide, and germanium sulfide were ball milled in a ball mill for 12 hours at a ratio of 5:2:1 (molar ratio), and heat-treated at 600°C for 6 hours to obtain a sulfur-based solid electrolyte. PVDF polymer and LiTFSI were mixed at a molar ratio of 30:1 , add sulfide powder and polymer / lithium salt into acetonitrile at a mass ratio of 1:1, stir magnetically at room temperature for 48 hours, remove the organic solvent by suction filtration, and dry at 50°C to obtain an organic / inorganic composite solid electrolyte. The coating layer of the organic polymer has a thickness of 100-120 nm and an ionic conductivity of ~10 at room temperature -3 S / cm.

[0056] The scanning electron microscope image of the organic / inorganic composite solid electrolyte material prepared in Example 2, Figure 4 The XRD pattern of the organic / inorganic composite solid electrolyte material prepared for example 2. Depend on image 3 , Figure 4 It can be seen that...

Embodiment 3

[0058] Lithium sulfide, phosphorus pentasulfide, and aluminum sulfide were ball milled in a ball mill for 16 hours at a ratio of 6:2:1 (molar ratio), and heat-treated at 400°C for 10 hours to obtain a sulfur-based solid electrolyte. PEO polymer and LiTFSI were mixed at a molar ratio of 5:1 , adding sulfide powder and polymer / lithium salt into tetrahydrofuran at a mass ratio of 150:1, stirring magnetically at room temperature for 36 hours, removing the organic solvent by suction filtration, and drying at 120°C to obtain an organic / inorganic composite solid electrolyte. The coating layer of organic polymer has a thickness of 5-10 nm and an ionic conductivity of ~10 at room temperature -5 S / cm.

[0059] The organic / inorganic composite solid-state electrolyte prepared in Example 1 was used to assemble an all-solid-state lithium-ion battery, and the elemental sulfur was used as the positive electrode, and metal lithium sheets were used to assemble an all-solid-state lithium-sulfur ...

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Abstract

The invention relates to an organic / inorganic composite solid electrolyte and a preparation method thereof. The sulfide is pretreated, the sulfide obtained by the pretreatment is subjected to high-temperature heat treatment to obtain a sulfur-based solid electrolyte, and the sulfur-based solid electrolyte is mixed with an organic polymer and a lithium salt in an organic solvent. The organic solvent is removed and the organic / inorganic composite solid electrolyte is obtained by drying. The inner layer of the organic / inorganic composite solid electrolyte material is a sulfur-based solid electrolyte, the organic polymer is coated on the outside of the sulfur-based solid electrolyte, the sulfur-based solid electrolyte has a structure of three phases or more, or an organic / inorganic composite electrolyte is composed of a two-phase sulfide solid electrolyte and a low-decomposition-temperature polymer organic matter, so that the activity of the obtained organic / inorganic composite solid electrolyte is improved, the conductivity is improved, and the cycle performance of the lithium-sulfur battery is improved.

Description

technical field [0001] The invention belongs to the technical field of new energy materials, and in particular relates to the preparation and application of a lithium-ion battery solid electrolyte. Background technique [0002] Lithium-ion batteries have the characteristics of high energy density, long cycle life, and no memory effect. They are widely used in daily consumer electronics, electric vehicles, and grid energy storage. At present, commercial lithium-ion batteries generally use organic liquid electrolytes and gel electrolytes. Liquid and gel electrolytes have high ionic conductivity, but because they contain volatile, flammable, and explosive organic solvents, they have serious safety hazards. question. Solid-state electrolytes can effectively solve the safety hazards of lithium-ion batteries caused by liquid electrolytes. At the same time, solid-state electrolytes can inhibit the generation of lithium dendrites during battery cycling, making it possible for metal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0562H01M10/0565H01M10/0525
CPCY02E60/10
Inventor 慈立杰徐小燕
Owner 深圳索理德新材料科技有限公司
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