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A kind of preparation method of submicron lithium negative electrode material

A sub-micron, lithium negative electrode technology, applied in battery electrodes, lithium batteries, structural parts, etc., can solve problems such as large median particle size of metal lithium powder, inability to prepare lithium powder, and increased safety hazards

Active Publication Date: 2020-07-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the high reactivity, high viscosity and good ductility of metal lithium itself make it difficult to synthesize micro-nanoscale metal lithium powders by mechanical pulverization and other common methods.
The currently adopted method of dispersing metal lithium powder in inert hydrocarbon oil after melting has the following problems: the operating temperature is high and needs to exceed the melting point of metal lithium; the molten metal lithium is highly corrosive and requires relatively harsh equipment; Hydrocarbon oil with high boiling point is used to disperse the droplets of molten lithium, and hydrocarbon oil with low boiling point is also required for washing lithium powder, resulting in large environmental pollution, cumbersome preparation methods, and low production yield; the median particle size of the prepared lithium metal powder is The diameter is still large, between 10-500μm, and it is impossible to prepare lithium powder below the micron scale
[0008] Although the above-mentioned preparation method can obtain metal lithium particles of submicron-nanometer size, if the relative content of lithium metal is high, the reduction of metal lithium particles and the improvement of chemical reactivity in the ultrasonic process will affect the safety of the system. The hidden dangers also increase, and the requirements for instruments and equipment are also more stringent, which is not conducive to actual production and application

Method used

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  • A kind of preparation method of submicron lithium negative electrode material
  • A kind of preparation method of submicron lithium negative electrode material
  • A kind of preparation method of submicron lithium negative electrode material

Examples

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Effect test

Embodiment 1

[0055] A method for preparing a submicron lithium negative electrode material, the specific contents are as follows:

[0056] (1) In a glove box of an argon atmosphere, 1 g of tetrabutylphosphine bis(trifluoromethanesulfonyl) imide salt ([P 444 ][NTf 2 ], melting point is 65°C) into a stainless steel ball mill jar, then heated to 150°C, and kept for 1 hour to remove moisture therein.

[0057] (2) [P] in the stainless steel ball mill jar 444 ][NTf 2 ] to 100°C, add 4 electrode-grade lithium sheets (mass about 0.32g) with a diameter of 15mm and a thickness of 0.7mm to form a [P 444 ][NTf 2 ] / lithium mixture.

[0058] (3) Place the stainless steel ball milling tank in the freezing medium liquid nitrogen to carry out the freezing ball milling; the mechanism of the freezing ball milling is: adopt the mode of vibratory ball milling, first pre-freeze for 15 minutes, and then carry out high-frequency ball milling, the frequency is 25Hz, and the time is 5 Minutes; then change to ...

Embodiment 2

[0084] (1) In dry air, mix 200mg of N-butyl-N-methylpyrrolidine bis(fluoromethanesulfonyl)imide salt ([C 4 mPyr + ][FSI - ]) centrifuge tube, and then heated to 130 ° C, and kept for 0.5 hours to remove the water.

[0085] (2) Then [C 3 mPyr + ][FSI - ] Cool down to 120° C., add 250 mg of lithium particles with a particle size of about 3 to 5 mm. After cooling to room temperature, the [C 3 mPyr + ][FSI - ] / lithium particle mixture is put into the ball milling tank, and the planetary freezing ball mill is used for freezing ball milling.

[0086] (3) Put the stainless steel ball milling tank in the planetary freezing ball mill, and carry out the freezing ball milling in the medium liquid nitrogen; the mechanism of the freezing ball milling is: adopt the method of planetary ball milling, pre-freeze for 30 minutes first, and then perform high-speed ball milling, The rotating speed is 400rpm, and the time is 15 minutes; then change to low-speed ball milling for intermediat...

Embodiment 3

[0089] (1) In a glove box of an argon atmosphere, 50 mL of N-butyl-N-methylpiperidine bis(trifluoromethanesulfonyl)imide salt ([Pp 14 + ][TFSI - ]) was added to a stainless steel bottle with a lid, and then heated to 200°C and kept for 8 hours to remove moisture therein.

[0090] (2) Then [Pp 14 + ][TFSI - ] cool down to 150°C, add 100mg of electrode-grade lithium flakes with a diameter of 15mm and a thickness of 0.7mm, cool to room temperature, and [C 3 mPyr + ][FSI - ] / lithium particle mixture is put into the ball mill tank, and the horizontal frozen ball mill is used to carry out frozen ball milling.

[0091] (3) Place the stainless steel ball milling tank in the freezing medium liquid nitrogen for freezing ball milling; the mechanism of freezing ball milling is: adopt the mode of planetary ball milling, first pre-freeze for 30 minutes, and then carry out high-speed ball milling, the rotating speed is 500rpm, and the time is 20 Minutes; then change to low-speed ball...

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Abstract

The invention discloses a preparation method of a submicron lithium negative electrode material. The method comprises the following steps of in inert gas or dry air atmosphere, mixing metal lithium raw materials with ion liquid to obtain a mixture; in freezing medium environment, performing freezing ball milling treatment on the mixture to obtain submicron metal lithium particles dispersed in ionliquid. The principle that metal lithium can realize embrittlement in freezing environment is used; the ion liquid containing metal lithium raw materials is put into the freezing medium environment for freezing ball milling treatment; therefore the ordinary sticky and strong-ductility metal lithium has strong brittleness; in a mechanical ball milling mode, the lithium with great particle dimensions is crushed into smaller particles; the preparation time of the metal lithium particles is shortened; the preparation efficiency of the metal lithium particles is improved; products with excellent electrochemical performance are also obtained.

Description

technical field [0001] The invention relates to the technical field of negative electrode materials for lithium secondary batteries, in particular to a preparation method for submicron lithium negative electrode materials. Background technique [0002] With the development of science and technology and the progress of human society, the problems of energy depletion and environmental pollution have become increasingly prominent. The development of new efficient and clean energy conversion, storage technologies and energy utilization methods has become the key to solving these problems and realizing the sustainable development of human society. Chemical power supply is an important technical approach to alleviate energy, resource and environmental crises, and plays an important role in the social energy system. [0003] Lithium is a silver-white metal with a very light texture (density 0.59g / cm 3 ), good ductility and conductivity. The theoretical specific capacity of metal ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/052
CPCH01M4/362H01M4/382H01M4/62H01M10/052Y02E60/10
Inventor 刘永锋蒲凯超潘洪革高明霞
Owner ZHEJIANG UNIV
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