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Powder pre-lithiated silicon-based negative electrode material, preparation method and application thereof

A pre-lithiated silicon-based, negative electrode material technology, applied in negative electrodes, battery electrodes, active material electrodes, etc., can solve the problems of reduced electronic conductivity and low first coulombic efficiency, so as to improve coulombic efficiency and improve cycle stability. , the effect of reducing consumption

Active Publication Date: 2019-09-06
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a powder pre-lithiated silicon-based negative electrode material and its preparation method and application, to solve the problem that the traditional silicon oxide material has a low initial Coulombic efficiency, and the partially lithiated silicon oxide is partially Lithium silicate and other by-products lead to technical problems such as a further reduction in the intrinsic electronic conductivity of the material

Method used

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  • Powder pre-lithiated silicon-based negative electrode material, preparation method and application thereof
  • Powder pre-lithiated silicon-based negative electrode material, preparation method and application thereof
  • Powder pre-lithiated silicon-based negative electrode material, preparation method and application thereof

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Embodiment 1

[0037] In an anhydrous and oxygen-free environment, take 1.25 L of butyllithium solution with a molar concentration of 0.8 mol / L (solvent is ether), add 2 mol of closed-type o-carborane (closo-1,2-C 2 B 10 h 12 ), reacted at 0°C for 12h, took 8 mol of silicon oxide (352g) with a D50 of 5μm, added to the above solution, soaked for 12h, and dried the above solution in a vacuum oven at 100°C to obtain a lithium-containing carborane cluster coating silicon oxide material. Place the silicon oxide material coated with lithium-containing carborane clusters in a rotary furnace under an argon atmosphere. The rotary furnace speed is 0.25r / min, and the temperature is kept at 400°C for 1h, then the temperature is raised to 1200°C, and the temperature is kept at 2h , cooled to room temperature and discharged to obtain a sintered material. Soak the sintered material in 10% dilute nitric acid solution for 3 hours, wash with deionized water until the solution is neutral, and filter and dry...

Embodiment 2

[0042] In an anhydrous and oxygen-free environment, take 2.4 L of methyllithium solution with a molar concentration of 2.5 mol / L (solvent is ether), add 2 mol of closed m-carborane (closo-1,7-C 2 B 10 h 12 ), reacted at -10°C for 1h, took 2mol of silicon oxide (88g) with a D50 of 7μm, added to the above solution, soaked for 12h, and dried the above solution in a vacuum oven at 80°C to obtain a lithium-containing carborane cluster clathrate coated silicon oxide material. Put the above silicon oxide material coated with lithium-containing carborane clusters in a rotary furnace under an argon atmosphere, the rotary furnace speed is 1r / min, and the temperature is kept at 200°C for 6h, then the temperature is raised to 800°C, and the temperature is kept at 12h , cooled to room temperature and discharged to obtain a sintered material. Soak the above-mentioned sintered material in 20% dilute hydrochloric acid solution for 0.5h, wash with deionized water until the solution is neutr...

Embodiment 3

[0048] In an anhydrous and oxygen-free environment, take 1.2L of butyllithium solution with a molar concentration of 2.5mol / L (the solvent is benzene), add 2mol of closed-type p-carborane (closo-1,12-C 2 B 10 h 12), reacted at 30°C for 4h, took 2 mol of silicon oxide (88g) with a D50 of 6μm, added to the above solution, soaked for 12h, and dried the above solution in a vacuum oven at 80°C to obtain a lithium-containing carborane cluster coating silicon oxide material. Put the above-mentioned dried lithium-containing carborane cluster-coated silicon oxide material in a rotary furnace under an argon atmosphere, the rotary furnace speed is 0.5r / min, the temperature is kept at 300°C for 4h, and then the temperature is raised to 900°C ℃, keep the temperature for 6 hours, cool down to room temperature and discharge to obtain the sintered material. Soak the sintered material in dilute sulfuric acid solution for 0.5h, wash with deionized water until the solution is neutral, and fil...

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Abstract

The invention discloses a powder pre-lithiated silicon-based negative electrode material, a preparation method and application thereof. A lithium-containing carborane cluster compound coated silicon monoxide material is firstly prepared and obtained, then through segmented heating sintering, boron element in a lithium-containing carborane cluster compound is diffused into a silicon-based materialcontinuously, a part of silicon atoms are replaced to form displaced doping, and the vacancy current-carrying concentration is improved, so that the intrinsic electronic conductivity of the silicon material is improved. Moreover, in the high temperature sintering process, incompletely reacted lithium ions inside the lithium-containing carborane cluster compound react with silicon monoxide, and thebyproducts such as lithium metasilicate, lithium silicate and lithium oxide are further formed to realize pre-lithiation, so that the initial coulomb efficiency of the battery prepared from the material is improved. And then, a uniformly compact carbon layer is formed on the surface of the material through chemical vapor deposition, and the defect that the carbon layer formed by the carbonizationof the carborane cluster compound is relatively loosened and porous can be solved, so that the cycling stability of the material is further improved.

Description

technical field [0001] The invention relates to a lithium-ion battery material, in particular to a powder pre-lithiated silicon-based negative electrode material and a preparation method and application thereof. Background technique [0002] With the development of electric vehicles and portable appliances, the demand for lithium-ion batteries with high energy density is also increasing. The theoretical specific capacity of traditional graphite anode materials is only 372mAh / g, which is difficult to meet market demand. The first gram capacity of silicon materials is 4200mAh / g, the lithium intercalation platform is higher, the earth's crust is abundant, and it is environmentally friendly, which has gradually attracted widespread attention of researchers. [0003] However, the volume expansion of silicon is as high as 300%. During the cycle, it will not only cause silicon to separate from the surrounding conductive carbon network to form "dead silicon", but also cause silicon...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/48H01M4/58H01M4/62H01M10/0525
CPCH01M4/366H01M4/628H01M4/624H01M4/625H01M4/483H01M4/5825H01M10/0525H01M2004/027Y02E60/10
Inventor 王辉王庆莉林少雄许家齐周勇岐丁楚雄
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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