IP Library Granted Patent US 9,567,227
Granted Patent B2
US 9,567,227 · App. 13/342,524 · Granted Feb 14, 2017

Process for producing silicon, silicon, and panel for solar cells

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Quick Facts
Patent No.
US 9,567,227
App. No.
13/342,524
Granted
Feb 14, 2017
Kind
B2
Abstract

A process for producing silicon which comprises: bringing molten silicon containing an impurity into contact with molten salt in a vessel to react the impurity contained in the molten silicon with the molten salt; removing the impurity from the system.

Claims (25)

1. A process for producing silicon, which comprises: bringing molten silicon containing an impurity into contact with molten salt in a vessel to react the impurity contained in the molten silicon with the molten salt; vaporizing said impurity and said molten salt; and removing said impurity and said molten salt from said vessel by evacuation,

wherein said impurity contained in the molten silicon at least includes boron and/or phosphorous and

wherein the step of vaporizing said impurity and said molten salt; and removing said impurity from said vessel is a step in which a reaction product obtained by reacting the impurity contained in the molten silicon with the molten salt is vaporized and removed

wherein said molten silicon is reacted with said molten salt until said molten salt is completely vaporized.

2. The process for producing silicon according to claim 1 , wherein the step of removing the impurity from the vessel is a step in which the impurity contained in the molten silicon is removed from the vessel together with an inert gas as a carrier gas.

3. The process for producing silicon according to claim 1 , wherein a lid for controlling the rate of vaporization of the molten salt or of the reaction product obtained by reacting the impurity contained in the molten silicon with the molten salt is disposed at an inner part or upper part of the vessel.

4. The process for producing silicon according to claim 1 , wherein the reaction between the impurity contained in the molten silicon and the molten salt is conducted by forming an interface between the liquid phase of the molten silicon and the liquid phase of the molten salt.

5. The process for producing silicon according to claim 1 , wherein the molten salt comprises at least one compound selected from the group consisting of halide salts of alkali metals, halide salts of alkaline earth metals, composite salts containing an alkali metal and a halogen, and composite salts containing an alkaline earth metal and a halogen.

6. The process for producing silicon according to claim 1 , wherein the molten salt comprises at least one compound selected from the group consisting of sodium fluoride (NaF), sodium silicofluoride (Na 2 SiF 6 ), cryolite (Na 3 AlF 6 ), mixtures of sodium fluoride and barium fluoride, and mixtures of sodium fluoride, barium fluoride, and barium chloride.

7. The process for producing silicon according to claim 1 , wherein an amount of the molten salt is 5-300% by weight based on the molten silicon.

8. The process for producing silicon according to claim 1 , wherein the impurity contained in the molten silicon is reacted with the molten salt while causing the molten silicon to flow by any one of the following methods (i) to (iv):

(i) a method of blowing an inert gas into the molten silicon,

(ii) a method of inductively stirring the molten silicon by using a high-frequency induction furnace,

(iii) a method of mechanically forcing the molten salt of an upper layer into the molten silicon of a lower layer,)

(iv) a method of stirring the molten silicon by using a rotor.

9. or producing silicon according to claim 1 , wherein the molten salt is continuously added to the molten silicon and the step of removing the impurity from the vessel is conducted by a continuous suction removal.

10. The process for producing silicon according to claim 1 , wherein after the step of removing the impurity from the vessel, molten salt is added to the molten silicon again and the step is conducted again.

11. The process for producing silicon according to claim 1 , wherein substances removed by the step of removing the impurity from the vessel are recovered to purify molten salt, and the purified molten salt is used again as molten salt.

12. The process for producing silicon according to claim 1 , wherein said molten silicon is obtained by heating and melting raw-material metal silicon, and said molten salt is added after heating and melting raw-material metal silicon.

13. The process for producing silicon according to claim 12 , wherein said raw material metal silicon and said molten salt are heated and melted at a temperature of 1450° C. or higher.

14. The process for producing silicon according to claim 1 , wherein said molten salt comprises at least one compound selected from the group consisting of a halide of an alkali metal and a composite salt comprising an alkali metal and a halogen, and an amount of molten salt is 10 to 300% by weight based on said molten silicon.

15. The process for producing silicon according to claim 1 , wherein a concentration of boron (B) in said molten silicon containing said impurity is 1.6 ppm or more, and a concentration of boron (B) in a silicon produced is 1.4 ppm or less.

16. The process for producing silicon according to claim 1 , wherein a period of contact between said molten silicon and said molten salt is 0.5 hours or longer.

17. The process for producing silicon according to claim 1 , wherein said molten silicon has a total concentration of impurity of 10 to 50 ppm.

18. The process for producing silicon according to claim 1 , wherein said molten silicon has a total concentration of impurity of 10 to 30 ppm.

Assignments (3)
CHANGE OF NAME Recorded Sep 5, 2017
From: MITSUBISHI RAYON CO., LTD.
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 043750/0834 →
MERGER Recorded Sep 4, 2017
From: MITSUBISHI CHEMICAL CORPORATION
To: MITSUBISHI RAYON CO., LTD.
Reel/Frame 043750/0207 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 3, 2012
From: ARITA, YOJI; YONEDA, TAKASHI
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 027471/0472 →