Submicron sized silicon powder with low oxygen content

Patent metadata

Field	Value
Publication number	US-10181600-B2
Application number	US-201113699004-A
Country	US
Kind code	B2
Filing date	Jun 22, 2011
Priority date	Jun 29, 2010
Publication date	Jan 15, 2019
Grant date	Jan 15, 2019

Abstract

A submicron sized Si based powder having an average primary particle size between 20 nm and 200 nm, wherein the powder has a surface layer comprising SiOx, with 0<x<2, the surface layer having an average thickness between 0.5 nm and 10 nm, and wherein the powder has a total oxygen content equal or less than 3% by weight at room temperature. The method for making the powder comprises a step where a Si precursor is vaporized in a gas stream at high temperature, after which the gas stream is quenched to obtain Si particles, and the Si particles are quenched at low temperature in an oxygen containing gas.

First claim

The invention claimed is:

1. A Si powder having an average primary particle size between 20 nm and 60 nm, wherein the powder comprises a surface layer consisting of SiO x , with 1≤x<2, the surface layer having an average thickness between 0.5 nm and 10 nm, and wherein the powder has a total oxygen content equal or less than 3% by-weight at room temperature.

2. The Si powder of claim 1 , wherein the surface layer has an average thickness between 0.5 nm and 5 nm.

3. A Si powder having an average primary particle size between 20 nm and 60 nm, wherein the powder has a SiO x surface layer, with 1≤x<2, the surface layer having an average thickness between 0.5 nm and 10 nm, and wherein the powder has a total oxygen content equal or less than 3% by-weight at room temperature, wherein the powder comprises at least 98% Si.

4. The Si powder of claim 1 , having a total oxygen content less than 4% by weight after being aged for 1 hour at 500° C. under atmospheric conditions and in air.

5. The Si powder of claim 1 , having a total oxygen content less than 5% by weight after being aged for 1 hour at 700° C. under atmospheric conditions and in air.

6. The Si powder of claim 1 , further comprising an element M selected from the group consisting of transition metals, metalloids, Group IIIa elements and carbon.

7. The Si powder of claim 6 , wherein M comprises either one of more elements selected from the group consisting of nickel, copper, iron, tin, aluminum and cobalt.

8. A Li-ion secondary battery comprising the Si powder of claim 1 as a negative electrode material.

9. A method for manufacturing the Si powder of claim 1 , comprising:
providing a Si precursor,
providing a gas stream at a temperature of at least 1727° C.,
injecting the Si precursor into the gas stream, thereby vaporizing the Si precursor,
quenching the gas stream carrying the vaporized Si precursor to a temperature below 1327° C., thereby obtaining Si particles,
passivating the Si particles in an oxygen containing gas at a temperature below 700° C., and
separating the Si particles from the gas stream after passivation.

10. The method of claim 9 , wherein passivation is performed at a temperature below 450° C.

11. The method of claim 10 , wherein passivation is performed at a temperature between room temperature and 100° C.

12. The method of claim 9 , wherein the gas stream is provided by a gas burner, a hydrogen burner, an RF plasma or a DC arc plasma.

13. The method of claim 9 , wherein passivation is performed in an oxygen containing gas comprising one or more additional components selected from the group consisting of Ar, N2, H2, CO and CO2.

14. The method of claim 13 , wherein the oxygen containing gas is a mixture of oxygen and nitrogen, with less than 1% oxygen by weight.

15. The method of claim 9 , wherein passivation is carried out for a period of less than 60 minutes.

16. The method of claim 15 , wherein passivation is carried out for a period of less than 10 minutes.

17. The method of claim 9 , wherein the gas stream is provided in a radio frequency inductively coupled plasma, and wherein the gas stream comprises argon gas.

Assignees

• Scoyer Jean
• Put Stijn
• Nelis Daniel
• Driesen Kris
• Umicore Nv

Inventors

• Scoyer Jean
• Put Stijn
• Nelis Daniël
• Driesen Kris

Classifications

• H01M2004/027

  Negative electrodes · CPC title

• C01B33/00 Primary

  Silicon; Compounds thereof ({C01B6/00,} C01B21/00, C01B23/00 take precedence; persilicates C01B15/14; carbides C01B32/956) · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01B33/03

  by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent · CPC title

• H01M2220/30

  Batteries in portable systems, e.g. mobile phone, laptop · CPC title