IP Library Granted Patent US 9,676,632
Granted Patent B2
US 9,676,632 · App. 14/409,536 · Granted Jun 13, 2017

Method for purifying silicon

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Quick Facts
Patent No.
US 9,676,632
App. No.
14/409,536
Granted
Jun 13, 2017
Kind
B2
Abstract

A method that includes: (a) forming a molten liquid from a solvent metal, silicon, and an alkali magnesium halide; (b) cooling the molten liquid to provide silicon crystals and a mother liquor; and (c) separating the silicon crystals from the mother liquor.

Claims (29)

1. A method comprising:

(a) forming a molten liquid from a solvent metal, a first silicon, and an alkali magnesium halide, wherein the solvent metal comprises at least one of copper, tin, zinc, antimony, silver, bismuth, aluminum, cadmium, gallium, indium, magnesium, lead, and alloys thereof, wherein the alkali magnesium halide is employed in at least about 0.10 wt. % of the molten liquid and up to about 10 wt. % of the molten liquid and the alkali magnesium halide comprises a combination of at least two of: synthetic carnallite; anhydrous carnallite; potassium magnesium chloride, KMgCl 3 , K 2 MgCl 4 , K 3 Mg 2 Cl 7 , Na 2 MgCl 4 , and MgNaCl 3 , and wherein the first silicon has a phosphorous level up to about 60 ppmw and a boron level up to about 15 ppmw;

(b) cooling the molten liquid to provide silicon crystals and a mother liquor; and

(c) separating the silicon crystals from the mother liquor;

wherein the silicon crystals are purified from phosphorous and boron compared to the first silicon.

2. The method of claim 1 , wherein the molten liquid is formed by contacting the solvent metal and the first silicon to form a mixture, heating the mixture to form a molten liquid, and then contacting the molten liquid with the alkali magnesium halide.

3. The method of claim 2 , wherein the alkali magnesium halide is contacted with the molten liquid at a bottom portion of the molten liquid by injecting the alkali magnesium halide into a bottom portion of the molten liquid.

4. The method of claim 1 , wherein the silicon crystals separated from the mother liquor comprise less than about 8 ppmw phosphorous without any further purification.

5. The method of claim 1 , wherein the silicon crystals separated from the mother liquor comprise less than about 5 ppmw boron without any further purification.

6. The method of claim 1 , wherein the cooling of the molten liquid to provide the silicon crystals and the mother liquor is carried out to a temperature above the solidus temperature.

7. The method of claim 1 , wherein the silicon crystals separated from the mother liquor comprise less than about 3,000 ppmw aluminum.

8. The method of claim 1 , wherein any one or more of steps (a)-(c) is repeated one or more times.

9. The method of claim 1 , wherein the mother liquor comprises at least about 1,000 ppmw aluminum.

10. A method comprising:

(a) forming a molten liquid from a solvent metal, silicon, and an alkali magnesium halide, wherein the alkali magnesium halide comprises a combination of KMgCl 3 , K 2 MgCl 4 , and K 3 Mg 2 Cl 7 ;

(b) cooling the molten liquid to provide silicon crystals and a mother liquor; and

(c) separating the silicon crystals from the mother liquor.

11. The method of claim 1 , wherein the alkali magnesium halide comprises potassium magnesium chloride as at least one of fine particles or a granular form.

12. The method of claim 1 , further comprising contacting the molten liquid with magnesium metal (Mg 0 ).

13. The method of claim 12 , wherein the magnesium metal is employed in at least about 0.1 wt. % of the molten liquid.

14. The method of claim 1 , further comprising contacting the molten liquid with at least one of MgCl 2 , KCl, and NaCl.

15. The method of claim 1 , wherein the silicon crystals are purified from phosphorous, such that at least about 25 wt. % of the phosphorous is removed from the first silicon.

16. The method of claim 1 , wherein the silicon crystals separated from the mother liquor comprise less than about 4 ppmw phosphorous and less than about 1 ppmw boron without any further purification.

17. The method of claim 1 , wherein the silicon crystals separated from the mother liquor are purified such that at least about 33 wt. % of the phosphorous from the first silicon is removed without any further purification.

18. A method comprising:

(a) forming a molten liquid from a solvent metal, a first silicon, and an alkali magnesium halide, wherein the alkali magnesium halide comprises a combination of two or more of YMgX 3 , Y 2 MgX 4 , and Y 3 Mg 2 X 7 , wherein X is a halide element and Y is an alkali element;

(b) cooling the molten liquid to provide silicon crystals and a mother liquor; and

(c) separating the silicon crystals from the mother liquor.

19. The method of claim 18 , wherein each X is independently selected from a chlorine (Cl) atom or a bromine (Br) atom and each Y is independent selected from a potassium (K) atom or a sodium (Na) atom.

Assignments (6)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 26, 2023
From: SUNNUVELLIR SLHF
To: HIGHLAND MATERIALS, INC.
Reel/Frame 064388/0757 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 25, 2023
From: SILICOR MATERIALS, INC.
To: SUNNUVELLIR SLHF
Reel/Frame 062511/0046 →
LIEN Recorded May 26, 2017
From: SILICOR MATERIALS, INC.
To: SCHWEGMAN, LUNDBERG & WOESSNER, P.A.
Reel/Frame 042592/0974 →
SECURITY INTEREST Recorded Dec 27, 2016
From: SILICOR MATERIALS, INC.
To: SUNNUVELLIR SLHF
Reel/Frame 040777/0104 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 18, 2016
From: MANCINI, PAUL A; TURENNE, ALAIN
To: SILICOR MATERIALS INC.
Reel/Frame 039176/0429 →
LICENSE Recorded Oct 13, 2015
From: SILICOR MATERIALS, INC.
To: SMS GROUP GMBH
Reel/Frame 036811/0327 →