IP Library Granted Patent US 11,261,096
Granted Patent B2
US 11,261,096 · App. 16/023,648 · Granted Mar 1, 2022

Controlled silicon polymer treatment method

Inventors: Matthias Colomb (Theodore, AL); Rick Deckbar (Theodore, AL); Bryan Nettles (Mobile, AL)
Assignees: Mitsubishi Polycrystalline Silicon America Corporation (MIPSA); MITSUBISHI MATERIALS CORPORATION
C01B33/12C01B33/035
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Quick Facts
Patent No.
US 11,261,096
App. No.
16/023,648
Granted
Mar 1, 2022
Kind
B2
Abstract

A polymer inactivation method for a polycrystalline silicon manufacturing device, wherein the polymer byproducts are treated and additionally treated in a manner that controls the rate of reaction. The polymer byproducts are treated with a first inert gas under partial vacuum and a second oxygen containing gas to convert the polymer byproducts. The reaction rate can be controlled by regulating the fill pressure of reactant gas, controlling the amount of oxygen in the reactant gas, and stripping of the raw polymer with heat and or a vacuum. The solid byproduct remaining after treating the polymer, which is predominately silicon suboxides (SiO x ) and silicon dioxide (SiO 2 ), is inert and is easily removed.

Claims (22)

1. A polymer inactivation method, comprising:

providing a sealable vessel containing silicon polymers which are a byproduct of a production of polycrystalline silicon in a Siemens process or a byproduct from a silicon epitaxy reactor, wherein the silicon polymers comprise non-hydrolyzed silicon polymers, hydrolyzed silicon polymers and partially-hydrolyzed silicon polymers;

sealing the sealable vessel to close the sealable vessel to prevent gas or fluid leaking from the sealable vessel;

filling the sealable vessel with an inert gas selected from the group consisting of nitrogen and argon;

pulling a partial vacuum on the sealable vessel; and

adding a second gas to the sealable vessel to cause a reaction between the second gas and the silicon polymer, wherein the second gas is selected from the group consisting of an oxygen containing gas for a reaction with non-hydrolyzed silicon polymers, and pure nitrogen for a reaction with hydrolyzed silicon polymers and partially-hydrolyzed silicon polymers;

whereby the silicon polymers are converted, in whole or in part, to silicon dioxide.

2. The polymer inactivation method of claim 1 , wherein the silicon polymers are selected from the group consisting of: hydrolyzed Si 2 Cl 6 , partially-hydrolyzed Si 2 Cl 6 , non-hydrolyzed Si 2 Cl 6 , hydrolyzed Si 2 HCl 5 , partially-hydrolyzed Si 2 HCl 5 , non-hydrolyzed Si 2 HCl 5 , hydrolyzed Si 2 H 2 Cl 4 , partially-hydrolyzed Si 2 H 2 Cl 4 , non-hydrolyzed Si 2 H 2 Cl 4 , hydrolyzed Si 3 Cl 8 , partially-hydrolyzed Si 3 Cl 8 , non-hydrolyzed Si 3 Cl 8 , hydrolyzed Si 4 Cl 10 , partially-hydrolyzed Si 4 Cl 10 , and non-hydrolyzed Si 4 Cl 10 .

3. The polymer inactivation method of claim 1 , further comprising a step of adding a third gas to the sealable vessel containing the partially-hydrolyzed silicon polymers, wherein the third gas is an oxygen containing gas.

4. The polymer inactivation method of claim 1 , further comprising adding an additional chemical to the sealable vessel to lower the pressure at which the reaction will occur.

5. The polymer inactivation method of claim 1 , wherein the conversion of silicon polymers to silicon dioxide is in an amount selected from the group consisting of: about 25%, about 50%, about 75% and about 100%.

6. A polymer inactivation method for a polycrystalline silicon manufacturing device, comprising:

providing the polycrystalline silicon manufacturing device containing silicon polymers which are a byproduct of a production of polycrystalline silicon in a Siemens process or a byproduct from a silicon epitaxy reactor, wherein the silicon polymers comprise non-hydrolyzed silicon polymers, hydrolyzed silicon polymers and partially-hydrolyzed silicon polymers;

sealing the polycrystalline silicon manufacturing device to close the polycrystalline silicon manufacturing device to prevent gas or fluid leaking from the polycrystalline silicon manufacturing device;

filling the polycrystalline silicon manufacturing device with an inert gas selected from the group consisting of nitrogen and argon;

pulling a partial vacuum on the polycrystalline silicon manufacturing device; and

adding a second gas to the polycrystalline silicon manufacturing device to cause a reaction between the second gas and the silicon polymer, wherein the second gas is selected from the group consisting of an oxygen containing gas for a reaction with non-hydrolyzed silicon polymers, and pure nitrogen for a reaction with hydrolyzed silicon polymers and partially-hydrolyzed silicon polymers;

whereby the silicon polymers are converted, in whole or in part, to silicon dioxide.

7. The polymer inactivation method of claim 6 , wherein the silicon polymers are selected from the group consisting of: hydrolyzed Si 2 Cl 6 , partially-hydrolyzed Si 2 Cl 6 , non-hydrolyzed Si 2 Cl 6 , hydrolyzed Si 2 HCl 5 , partially-hydrolyzed Si 2 HCl 5 , non-hydrolyzed Si 2 HCl 5 , hydrolyzed Si 2 H 2 Cl 4 , partially-hydrolyzed Si 2 H 2 Cl 4 , non-hydrolyzed Si 2 H 2 Cl 4 , hydrolyzed Si 3 Cl 8 , partially-hydrolyzed Si 3 Cl 8 , non-hydrolyzed Si 3 Cl 8 , hydrolyzed Si 4 Cl 10 , partially-hydrolyzed Si 4 Cl 10 , and non-hydrolyzed Si 4 Cl 10 .

8. The polymer inactivation method of claim 6 , further comprising a step of adding a third gas to the polycrystalline silicon manufacturing device containing the partially-hydrolyzed silicon polymers, wherein the third gas is an oxygen containing gas.

9. The polymer inactivation method of claim 6 , further comprising adding an additional chemical to the polycrystalline silicon manufacturing device to lower the pressure at which the reaction will occur.

10. The polymer inactivation method of claim 6 , wherein the conversion of silicon polymers to silicon dioxide is in an amount selected from the group consisting of: about 25%, about 50%, about 75% and about 100%.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 5, 2023
From: MITSUBISHI MATERIALS CORPORATION
To: HIGH-PURITY SILICON CORPORATION
Reel/Frame 063858/0867 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 9, 2018
From: COLOMB, MATTHIAS; DECKBAR, RICK; NETTLES, BRYAN
To: MITSUBISHI POLYCRYSTALLINE SILICON AMERICA CORPORATION (MIPSA); MITSUBISHI MATERIALS CORPORATION
Reel/Frame 047104/0978 →
Continuity (2)
Provisional Application 62527505 · Jun 30, 2017
Related Publication 20190002296A1 · Jan 3, 2019