System for reducing oxygen contamination of milled silicon

• US 10,569,278 B1
• Filed: 10/11/2019
• Issued: 02/25/2020
• Est. Priority Date: 10/02/2019
• Status: Active Grant

• Current Assignee: Advano
• Original Assignee: Nanostar Inc.
• Inventors: Goodman, Jonathan, Marus, Gregory Alan
• Primary Examiner(s): Swiatocha, Gregory D
• Application Number:
  US16/599,219
• Time in Patent Office: 137 Days
• CPC Class Codes: B02C 21/00 Disintegrating plant with or without drying of the material for grain B02C9/04
• CPC Class Codes: B02C 23/08 Separating or sorting of material, associated with crushing or disintegrating B02C23/18 takes precedence ; beater mills combined with sifting devices B02C13/13, B02C13/14; for tumbling mills B02C17/1835
• CPC Class Codes: B02C 23/18 Adding fluid, other than for crushing or disintegrating by fluid energy for tumbling mills B02C17/186; feeding devices B02C23/02
• CPC Class Codes: B29B 13/10 by grinding, e.g. by triturating; by sieving; by filtering
• CPC Class Codes: C01B 33/02 Silicon forming single crystals or homogeneous polycrystalline material with defined structure C30B

Abstract

A milling system which includes a reservoir shaped and sized to contain a solvent or a slurry including the solvent and a material to be milled, a treatment column in communication with the reservoir, wherein the treatment column is configured to remove one or more of water, oxygen, and/or other impurities from the solvent, and a mill in fluid communication with the reservoir, wherein the mill is configured to triturate the material. The treatment column may be fluidly isolated from the rest of the system during milling.

Claims

1. A milling system, comprising:

a reservoir shaped and sized to carry a solvent or a slurry comprising the solvent and a material to be milled;

a treatment column in communication with the reservoir, the column configured to remove one or more of water, oxygen, or impurities from the solvent; and

a mill in fluid communication with the reservoir, the mill configured to triturate the material when carried in the solvent;

wherein the treatment column is disposed before the mill relative to a drying-process flow through the milling system.

2. The milling system of claim 1, wherein the mill is configured to mechanochemically functionalize a surface of the material to be milled.

3. The milling system of claim 1, wherein the milling system is configured to re-circulate the solvent through the reservoir, the treatment column, and the mill.

4. The milling system of claim 3, wherein the system includes a recirculation pump configured to circulate the solvent or the slurry to the mill and return the solvent or the slurry to the reservoir.

5. The milling system of claim 1, wherein the treatment column is configured to be fluidly, selectively isolated from the reservoir and the mill.

6. The milling system of claim 1, wherein the treatment column includes a desiccant.

7. The milling system of claim 6, wherein the desiccant are molecular sieves.

8. The milling system of claim 6, wherein the treatment column is configured for regeneration of the desiccant.

9. The milling system of claim 6, wherein the desiccant is adapted to reduce an amount of water from the solvent;

wherein the solvent includes one or more of an alkane, an alkene, an alkyne, an arene, an alkyl halide, an aryl halide, an aldehyde, a ketone, an ester, an amide, an amine, and a nitrile.

10. A method comprising:

providing a nonaqueous solvent;

circulating the solvent through a mill and a treatment column configured to remove water from the solvent;

monitoring or calculating an amount of water in the solvent; and

thereafter

operating the mill to triturate a material to be milled.

11. The method of claim 10, wherein said circulating further includes circulating the solvent through a reservoir shaped and sized to carry a slurry comprising the solvent and the material to be milled.

12. The method of claim 10, wherein circulating the solvent through the mill and the treatment column dries the mill;

and drying the solvent to below a selected amount of water in the solvent.

13. The method of claim 12, further comprising, after drying the mill,

introducing to the mill a slurry that includes the material to be milled;

and

triturating the material in the mill.

14. The method of claim 10, comprising isolating the treatment column from the mill and a reservoir during operation of the mill.

15. The method of claim 10, further comprising introducing to the mill a slurry including the material to be milled;

and circulating the slurry through the treatment column during operation of the mill.

16. The method of claim 10, wherein the solvent includes one or more of an alkane, an alkene, an alkyne, an arene, an alkyl halide, an aryl halide, an aldehyde, a ketone, an ester, an amide, an amine, or a nitrile.

17. The method of claim 10, wherein the solvent includes an alkane, an alkene, an alkyne, or an arene.

18. A method of operating a mill, comprising:

providing a nonaqueous solvent;

circulating the solvent through the mill and a treatment column configured to remove water from the solvent;

reducing an amount of water in the solvent to less than about 1000 ppm;

then introducing a material to be milled into the solvent to produce a slurry; and

operating the mill to triturate the material.

19. The method of claim 18, wherein said operating comprises:

a) pumping the slurry from a first reservoir into the mill;

b) milling the slurry in the mill;

c) pumping the slurry into a second reservoir;

d) pumping the slurry from the second reservoir into the mill;

e) milling the slurry in the mill;

f) pumping the slurry into the first reservoir; and

g) repeating a-f until the material in the slurry is milled to a predetermined specification.

20. The method of claim 18, wherein said circulating further includes circulating the solvent through at least one reservoir shaped and sized to carry the slurry comprising the solvent and the material to be milled.