Particulate anode materials and methods for their preparation

Patent metadata

Field	Value
Publication number	US-9559355-B2
Application number	US-201214345786-A
Country	US
Kind code	B2
Filing date	Sep 19, 2012
Priority date	Sep 19, 2011
Publication date	Jan 31, 2017
Grant date	Jan 31, 2017

Abstract

Method for preparing a particulate material including particles of an element of group IVa, an oxide thereof or an alloy thereof, the method including: (a) dry grinding particles from an ingot of an element of group IVa, an oxide thereof or an alloy thereof to obtain micrometer size particles; and (b) wet grinding the micrometer particles dispersed in a solvent carrier to obtain nanometer size particles having a size between 10 to 100 nanometers, optionally a stabilizing agent is added during or after the wet grinding. Method can include further steps of (c) drying the nanometer size particles, (d) mixing the nanometer size particles with a carbon precursor; and (e) pyrolyzing the mixture, thereby forming a coat of conductive carbon on at least part of the surface of the particles. The particulate material can be used in fabrication of an anode in an electrochemical cell or electrochemical storage energy apparatus.

First claim

The invention claimed is:

1. A method for preparing a particulate material comprising particles of silicon or an oxide thereof, the method comprising:
(a) dry grinding particles from an ingot of silicon or an oxide thereof to obtain micrometer size particles; and
(b) wet grinding the micrometer particles dispersed in a solvent carrier to obtain nanometer size particles having a size between 10 to 100 nanometers, optionally a stabilizing agent is added during or after the wet grinding;
wherein the ingot comprises at least 98% of silicon or an oxide thereof.

2. A method according to claim 1 , further comprising a step of (c) drying the nanometer size particles.

3. A method according to claim 2 , further comprising the steps of: (d) mixing the nanometer size particles with a carbon precursor; and (e) pyrolysing the mixture, thereby forming a coat of conductive carbon on at least part of the surface of the particles.

4. A method according to claim 3 , wherein the conductive carbon formed is non-powdery, and is in an amount of about 0.5-10% wt of the particulate material.

5. A method according to claim 3 , wherein step (e) is performed at a temperature of about 600-800° C.

6. A method according to claim 3 , wherein step (e) is performed at a rate of about 3-10° C./min.

7. A method according to claim 3 , wherein step (e) is performed during a period of about 30 minutes to 2 hours.

8. A method according to claim 3 , wherein step (e) is performed under inert atmosphere.

9. A method according to claim 1 , wherein step (a) is performed in a bead mill, a puck and ring mill, a jet mill or a cyclone mill.

10. A method according to claim 1 , wherein the carrier solvent is an organic solvent selected from the group consisting of isopropanol and cyclohexane, or is water.

11. A method according to claim 1 , wherein an amount of the solvent carrier is adjusted such as to represent about 5-20% wt of the particulate material.

12. A method according to claim 1 , wherein the carbon precursor is selected from the group consisting of an organic material, a cross-linkable monomer, oligomer, polymer and copolymer.

13. A method according to claim 1 , wherein the carbon precursor is poly(maleic anhydride-1-alt-octadecene).

14. A method according to claim 1 , wherein the stabilizing agent is a surfactant.

15. A method according to claim 1 , wherein the particulate material is used as an anode in an electrochemical cell or an electrochemical storage energy apparatus selected from the group consisting of a lithium-ion battery, a silicon-air battery and a polymer battery.

16. A method for preparing a particulate material comprising particles of silicon or an oxide thereof, the method comprising:
(a) dry grinding particles from an ingot of silicon or an oxide thereof to obtain micrometer size particles;
(b) wet grinding the micrometer particles dispersed in a solvent carrier to obtain nanometer size particles having a size between 10 to 100 nanometers, optionally a stabilizing agent is added during or after the wet grinding;
(c) mixing the nanometer size particles with a carbon precursor; and
(d) pyrolysing the mixture, thereby forming a coat of conductive carbon on at least part of the surface of the particles;
wherein the ingot comprises at least 98% of silicon or an oxide thereof.

17. A method according to claim 16 , wherein the method comprises drying the nanometer size particles.

Assignees

• Hydro Quebec
• HYDRO-QUéBEC

Inventors

• Zaghib Karim
• Guerfi Abdelbast
• Leblanc Dominic

Classifications

• H01M4/134

  Electrodes based on metals, Si or alloys · CPC title

• H01M4/366 Primary

  as layered products · CPC title

• H01M4/0471

  involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title

• H01M4/625

  Carbon or graphite · CPC title

• H01M4/1395

  of electrodes based on metals, Si or alloys · CPC title