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Method for preparing nano silicon through three-stage grinding

A technology of nano-silicon and grinding time, which is applied in the direction of nano-technology, silicon, structural parts, etc., can solve the problems of affecting the connection between active materials and current collectors, reversible capacity depletion, and difficulty in reaching a smaller size, so as to ensure uniform dispersion and stability performance, improve wet grinding efficiency, and reduce nano-silicon particle size

Pending Publication Date: 2020-05-19
MAANSHAN KEDA PURUI ENERGY TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Silicon has an ultra-high theoretical specific capacity (4200mAh / g) and a low delithiation potential (<0.5V), but the volume change of silicon can be as high as 300% during charge and discharge, which will cause silicon particles to break and affect the active material and assembly. The connection between fluids is not conducive to electron transmission; on the other hand, the solid electrolyte interface film formed between the silicon-based material and the electrolyte gradually thickens, resulting in a sharp decline in the cycle performance of lithium batteries
There are even studies that show that the first Coulombic efficiency of micron-sized silicon powder is less than 40%, and the cycle performance is very poor, and the reversible capacity is almost zero in less than 10 weeks.
In order to reduce the volume expansion of silicon particles, the most effective method is to nano-size silicon particles to reduce their absolute volume expansion. However, at this stage, the size of nano-silicon prepared by wet grinding is basically about 80-100nm, and it is difficult to achieve a smaller size.

Method used

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  • Method for preparing nano silicon through three-stage grinding

Examples

Experimental program
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Effect test

Embodiment 1

[0023] A method for preparing nano-silicon by three-stage grinding described in this embodiment is specifically carried out according to the following steps:

[0024] 1) Add high-purity silicon powder with a median particle size of 10 μm and a purity of ≥99% into the dispersion tank of a horizontal sand mill, add absolute ethanol to adjust the solid content to 40wt.%, and then add sodium pyrophosphate as a dispersant , wherein the mass ratio of sodium pyrophosphate to silicon powder is 10:100, pre-dispersed; the dispersed mixed solution is introduced into a horizontal sand mill for primary grinding, the line speed of the sand mill is 12m / s, and the zirconia The diameter of the ball is 1 μm, the ball-to-material ratio is 5:1, and the grinding time is 2 hours to obtain a particle size of nano-silicon D50<1000nm;

[0025] 2) Import the slurry after primary grinding into a horizontal sand mill for secondary grinding. The linear speed of the sand mill is 14m / s, the diameter of the ...

Embodiment 2

[0028] A method for preparing nano-silicon by three-stage grinding described in this embodiment is specifically carried out according to the following steps:

[0029] 1) Add high-purity silicon powder with a median particle size of 50 μm and a purity of ≥99% into the dispersion tank of a horizontal sand mill, add methanol to adjust the solid content to 30wt.%, and then add sodium acrylate as a dispersant, of which acrylic acid The mass ratio of sodium to silicon powder is 5:100 for pre-dispersion; the dispersed mixed solution is introduced into a horizontal sand mill for primary grinding, the line speed of the sand mill is 12.5m / s, and the diameter of the stainless steel ball is 5μm, the ball-to-material ratio is 8:1, the grinding time is 5h, and the particle size D50 of nano-silicon is <1000nm;

[0030] 2) Import the slurry after primary grinding into a horizontal sand mill for secondary grinding. The linear speed of the sand mill is 14.5m / s, the diameter of the stainless ste...

Embodiment 3

[0033] A method for preparing nano-silicon by three-stage grinding described in this embodiment is specifically carried out according to the following steps:

[0034] 1) Add high-purity silicon powder with a median particle size of 100 μm and a purity of ≥99% into the dispersion tank of a horizontal sand mill, add acetone to adjust the solid content to 20wt.%, and then add guar gum as a dispersant. The mass ratio of Gur gum to silica powder is 1:100, and the pre-dispersion is carried out; the dispersed mixed solution is introduced into a vertical sand mill for primary grinding, and the line speed of the sand mill is 13m / s. The diameter is 10 μm, the ball-to-material ratio is 10:1, the grinding time is 10 hours, and the particle size D50<1000nm of nano-silicon is obtained;

[0035] 2) Import the slurry after primary grinding into a vertical sand mill for secondary grinding. Time 30h, obtain nano-silicon particle size D50<100nm;

[0036] 3) Import the slurry after the secondar...

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Abstract

The invention belongs to the field of nano material preparation, and particularly discloses a method for preparing nano silicon through three-stage grinding. The method comprises the following steps:1) adding high-purity silicon powder, a solvent and a dispersing agent into a dispersing tank of a first-stage sand mill, and carrying out pre-dispersion; introducing the dispersed mixed solution intoa first-stage sand mill for first-stage grinding to obtain silicon slurry with the nano-silicon particle size D50 of less than 1000nm; (2) introducing the slurry subjected to primary grinding into asecond-stage sand mill for secondary grinding to obtain silicon slurry with the nano-silicon particle size D50 of less than 100nm; (3) introducing the slurry subjected to secondary grinding into a third-stage sand mill for third-stage grinding to obtain silicon slurry with the nano-silicon particle size D50 of less than 50nm, and carrying out drying to obtain nano-silicon powder. Compared with theprior art, the method disclosed by the invention is simple in preparation process and low in cost, greatly improves the wet grinding efficiency, reduces the particle size of the nano silicon, ensuresthe uniform dispersity and stability of the silicon slurry, and is suitable for industrialization.

Description

technical field [0001] The invention belongs to the field of nanometer material preparation, and in particular relates to a method for preparing nanometer silicon by three-stage grinding. Background technique [0002] Silicon has an ultra-high theoretical specific capacity (4200mAh / g) and a low delithiation potential (<0.5V), but the volume change of silicon can be as high as 300% during charge and discharge, which will cause silicon particles to break and affect the active material and assembly. The connection between the fluids is not conducive to electron transport; on the other hand, the solid electrolyte interfacial film formed between the silicon-based material and the electrolyte gradually thickens, resulting in a sharp decline in the cycle performance of the lithium battery. There are even studies that show that the first coulombic efficiency of micron-sized silicon powder is less than 40%, and the cycle performance is very poor, and the reversible capacity is alm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/38C01B33/02B82Y40/00
CPCH01M4/386C01B33/02B82Y40/00Y02E60/10
Inventor 胡亮张少波张志权李晓马俞有康
Owner MAANSHAN KEDA PURUI ENERGY TECH CO LTD
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