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Method for grinding silicon-containing solids

A solid and gas technology, applied in chemical instruments and methods, silicon, silicon compounds, etc., can solve problems such as silicon consumption, silicon particles are no longer applicable, and achieve high efficiency.

Active Publication Date: 2019-06-18
WACKER CHEM GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Against this background, there is a concern that the milling of silicon-containing solids according to the invention proceeds so vigorously that dust explosions or reactions with reactive gases consume the silicon to such an extent that the obtained silicon particles are no longer suitable for the respective application , such as Li-ion batteries to the extent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1a

[0084] 5 kg of ultra-high purity polysilicon powder (Wacker BGF(sg) type PCL-NCS-F, d 10 = 100 μm, d 50 = 240 μm, d 90 =440 μm) into the storage tank of a fluidized bed jet mill CGS 16 (manufacturer: NetzschTrockenmahltechnik GmbH). The grinder is used at 20°C and 7 bar gauge pressure (oxygen partial pressure: 1.7 bar) with 48m 3 / h air operation. The speed of the classifier impeller was 3000 rpm.

[0085] After 150 minutes, stop the grinder and open the collection container on the particle filter. It contains 2.1kg of d 10 = 2.5 μm, d 50 = 4.5 μm and d 90 Silicon powder = 7.3 μm (measured in Horiba LA950). The surface area calculated from the particle size distribution under the assumption of spherical particles is 0.67m 2 / g. The pellets were stored in air at room temperature and ambient pressure. Then the oxygen content measured by Leco TCH600 oxygen analyzer is 0.43wt% or 6.5mg / m 2 (based on calculated particle surface area).

Embodiment 1b

[0087] During grinding as in Example 1a, the speed of the classifying wheel was increased to 8000 rpm. After 190 minutes, stop the grinder and open the collection container on the particle filter. It contains 450g of d 10 = 1.1 μm, d 50 = 2.7 μm and d 90 = 4.9 μm (measured in Horiba LA950) silicon powder. The surface area calculated from the particle size distribution under the assumption of spherical particles is 1.38m 2 / g. The pellets were stored in air at room temperature and ambient pressure. Then the oxygen content measured by Leco TCH 600 oxygen analyzer is 1.02wt% or 7.4mg / m 2 (based on calculated particle surface area).

Embodiment 2

[0089] 5 kg of ultra-high purity polysilicon powder (Wacker BGF(sg) type PCL-NCS-F, d 10 = 100 μm, d 50 = 240 μm, d 90 =440 μm) into the storage tank of a fluidized bed jet mill CGS 16 (manufacturer: NetzschTrockenmahltechnik GmbH). The grinder is used at 203°C and 3.2 bar gauge pressure (oxygen partial pressure: 0.9 bar) with 97m 3 / h air operation. The speed of the classifier impeller was 8000 rpm. After 60 minutes, stop the grinder and open the collection container on the particle filter. It contains 270g of d 10 = 1.3 μm, d 50 = 2.9 μm and d 90 = 5.0 μm (measured in Horiba LA950) silicon powder. The surface area calculated from the particle size distribution under the assumption of spherical particles is 1.2m 2 / g. The pellets were stored in air at room temperature and ambient pressure. Then the oxygen content measured by Leco TCH 600 oxygen analyzer is 1.03wt% or 8.6mg / m 2 (based on calculated particle surface area).

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Abstract

The invention relates to methods for producing silicon particles by grinding silicon-containing solids, wherein one or more gases are used, which contain reactive gas at a partial pressure of not lessthan 0.3 bar, wherein reactive gases are selected from the group comprising oxygen, ozone, inorganic peroxides, carbon monoxide, carbon dioxide, ammonia, nitrogen oxides, hydrogen cyanide, hydrogen sulfide, sulfur dioxide, and volatile organic compounds.

Description

technical field [0001] The present invention relates to a method for grinding silicon-containing solids. Background technique [0002] In many applications it is desirable to have silicon particles with a particle size in the micron range, for example when silicon particles are used as active material in the negative electrode of lithium-ion batteries. One way of producing such particles is by comminuting larger silicon particles, for example by grinding. In order to produce silicon powder with an average particle size of, for example, 0.02 to 10 μm, wet grinding methods are often used, as known from EP 3027690. In wet grinding methods, the material being ground is suspended in a grinding liquid. Abrasive fluids such as alcohols can react with silicon surfaces and release hydrogen gas. After wet milling, drying and thus additional steps are required to produce dry powders. A disadvantage is that the drying of the grinding suspension may involve agglomeration of silicon p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/02B02C17/00B22F9/00C09C1/28H01M4/134
CPCC01B33/02C09C1/28H01M4/134C01P2004/61C01P2004/62H01M4/386H01M4/58Y02E60/10C01B33/021H01M4/04H01M4/139H01M2004/028B01J2/16C01P2004/32C01P2004/52C01P2006/12C01P2006/40H01M2004/027
Inventor 埃克哈德·哈内尔特米夏埃尔·弗里克
Owner WACKER CHEM GMBH
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