Tapered fluidized bed reactor and process for its use

• US 10,265,671 B2
• Filed: 10/04/2018
• Issued: 04/23/2019
• Est. Priority Date: 08/29/2012
• Status: Active Grant

• Current Assignee: Hemlock Semiconductor | Hemlock Semiconductor Operations LLC
• Original Assignee: Hemlock Semiconductor | Hemlock Semiconductor Operations LLC
• Inventors: Bucci, John V., Cocco, Raymond Anthony, Dehtiar, Max E., Harder, Patrick J., Karri, S. B. Reddy, Knowlton, Ted M., Molnar, Michael J.
• Primary Examiner(s): Do, An H
• Application Number:
  US16/151,520
• Publication Number:
  US 20190030506A1
• Time in Patent Office: 201 Days
• CPC Class Codes: B01J 2208/00672 Particle size selection
• CPC Class Codes: B01J 2208/00752 Feeding
• CPC Class Codes: B01J 2208/00761 Discharging
• CPC Class Codes: B01J 2208/00902 Nozzle-type feeding elements
• CPC Class Codes: B01J 2208/00938 Flow distribution elements
• CPC Class Codes: B01J 2208/00982 Particulate material
• CPC Class Codes: B01J 2208/00991 Disengagement zone in fluidised-bed reactors
• CPC Class Codes: B01J 8/1827 the fluidising gas being a reactant
• CPC Class Codes: B01J 8/1836 Heating and cooling the reactor B01J8/42 takes precedence
• CPC Class Codes: B01J 8/1872 Details of the fluidised bed reactor B01J8/1836 takes precedence
• CPC Class Codes: B01J 8/24 according to "fluidised-bed" technique B01J8/20 takes precedence
• CPC Class Codes: B01J 8/44 Fluidisation grids
• CPC Class Codes: C01B 33/027 by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
• CPC Class Codes: C01B 33/03 by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
• CPC Class Codes: G01N 15/0255 with mechanical, e.g. inertial, classification, and investigation of sorted collections with centrifuges G01N15/042

Abstract

A fluidized bed reactor includes a gas distributor, a tapered section above the gas distributor, and an expanded head above the tapered section. The gas distributor defines a plurality of inlets surrounding a product withdrawal tube, which extends away from the fluidized bed reactor. The fluidized bed reactor is useful in a process for fluidizing relatively large particles, such as Geldart Group B particles and/or Geldart Group D particles, where said particles are in a bubbling fluidized bed residing, in whole or in part, in the tapered section. The fluidized bed reactor and process may be used for manufacturing polycrystalline silicon.

Claims

1. A process for preparing polycrystalline silicon in a fluidized bed reactor, where the process comprises:

feeding gases comprising hydrogen and a silicon bearing source gas comprising a silicon monomer into a bubbling fluidized bed containing silicon particles, where at least a portion of the bubbling fluidized bed resides in a tapered section of the fluidized bed reactor, where the tapered section expands upward and outward at a cone angle from vertical;

feeding silicon particles into the fluidized bed reactor above the tapered section;

heating the fluidized bed reactor, thereby causing thermal decomposition of the silicon monomer to produce polycrystalline silicon on surfaces of the silicon particles, thereby producing larger diameter particles; and

removing the larger diameter particles from the fluidized bed reactor.

2. The process of claim 1, where the cone angle ranges from 2.5°

to 10.0°

.

3. The process of claim 1, where the silicon bearing source gas comprises HSiCl₃ and optionally SiCl₄.

4. The process of claim 1, where the silicon bearing source gas comprises HSiBr₃ and optionally SiBr₄.

5. The process of claim 1, where the silicon bearing source gas comprises SiH₄.

6. The process of claim 1, wherein

a. the fluidized bed reactor further comprises a gas distributor located beneath the tapered section, where

i. a product withdrawal tube is mounted to the gas distributor,

ii. the gas distributor defines a plurality of feed inlets, and

iii. the feed inlets are located between the product withdrawal tube and an outer edge of the gas distributor, and

b. the silicon bearing source gas is fed into the fluidized bed reactor through the feed inlets, and

c. the larger diameter particles are removed from the fluidized bed reactor through the product withdrawal tube.

7. The process of claim 6, where all, or a portion, of the hydrogen is fed into the fluidized bed reactor through the product withdrawal tube.

8. The process of claim 6, where the gas distributor has a conical shape, which decreases in diameter going downward, and the product withdrawal tube is mounted to a lowermost portion of the gas distributor.

9. The process of claim 6, where the gas distributor has at least 2 feed inlets.

10. The process of claim 9, where the gas distributor has at least 4 feed inlets.

11. The process of claim 6, where the gas distributor further comprises a plurality of gas inlets, where the gas inlets are located between the feed inlets and the outer edge of the gas distributor, and where an etching gas is fed into the fluidized bed reactor through the gas inlets.

12. The process of claim 11, where the etching gas comprises HCl or SiCl₄.

13. The process of claim 11, where the etching gas comprises HBr or SiBr₄.

14. The process of claim 1, where the fluidized bed reactor further comprises an accelerometer.

15. The process of claim 14, wherein the process further comprises monitoring vibrations of the fluidized bed reactor with the accelerometer to determine a Sauter mean particle size distribution of the larger diameter particles.