US4826668A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for the production of ultra high purity polycrystalline silicon
Assignee: Advanced Silicon Materials LLC
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Filing: 1987-06-11
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Granted: 1989-05-02
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Expires: 2007-06-11
Abstract
Abstract The present invention is directed to an improved process for producing ultra high purity polycrystalline silicon which process provides for increased production capacity and electrical power efficiency. The process comprises recycling the exhaust gases of the silane pyrolysis reactor after the gases have been preferably first cooled and filtered utilizing a pocket-type reaction zone enclosure having a particular effective radius thereby effectively decreasing the amount of silicon powder formation. Preferably, the rate of recycle flow is sufficient to entrain silicon powder in the reactor and remove the powder from the reactor with the exiting exhaust gases.
Inventors
- 👤 William C. Breneman
- 👤 Robert N. Flagella
- 👤 Jon M. Gaston
- 👤 David W. Hagan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 03:21
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/02; C01B33/021; C01B33/027; C01B33/035
Claims Analysis
Total Claims: 31
Claim 1
Independent Claim
228 words
A process for the formation of polysilicon crystal rods in which the formation of silicon powder is reduced comprising: (a) providing an elongated starter rod substantially in the center of a cooled enclosure which enclosure has a wall at an effective radius of from about 6 cm. to 23 cm. and an upper outlet and a lower inlet; (b) energizing the starter rod while introducing silane into the cooled enclosure, said starter rod being maintained at a temperature sufficient to effect silicon decomposition and deposition thereon and forming a thermal boundary layer around the periphery of said rod and produce by homogeneous decomposition silicon powder, said silane being provided at a rate sufficient to maintain the silane concentration in the cooled enclosure in an amount of at least about 0.5 mole percent; and (c) continuing step (b) for a time sufficient to grow a silicon rod having a diameter no greater than about 80 to 90% of the diameter of the enclosure, and while growing said rod: (i) maintaining the wall of the enclosure at a temperature below about 100° C.; (ii) removing at least a portion of an effluent comprised of unreacted silane, silicon powder and by-product hydrogen from the upper outlet of the enclosure; and (iii) recycling the effluent at a rate of at least about 50,000 cubic cm./min. to the lower inlet of the enclosure.
Claim 2
Dependent Claim
228 words
A process for the formation of polysilicon crystal rods in which the formation of silicon powder is reduced comprising: (a) providing an elongated starter rod substantially in the center of a cooled enclosure which enclosure has a wall at an effective radius of from about 6 cm. to 23 cm. and an upper outlet and a lower inlet; (b) energizing the starter rod while introducing silane into the cooled enclosure, said starter rod being maintained at a temperature sufficient to effect silicon decomposition and deposition thereon and forming a thermal boundary layer around the periphery of said rod and produce by homogeneous decomposition silicon powder, said silane being provided at a rate sufficient to maintain the silane concentration in the cooled enclosure in an amount of at least about 0.5 mole percent; and (c) continuing step (b) for a time sufficient to grow a silicon rod having a diameter no greater than about 80 to 90% of the diameter of the enclosure, and while growing said rod: (i) maintaining the wall of the enclosure at a temperature below about 100° C.; (ii) removing at least a portion of an effluent comprised of unreacted silane, silicon powder and by-product hydrogen from the upper outlet of the enclosure; and (iii) recycling the effluent at a rate of at least about 50,000 cubic cm./min. to the lower inlet of the enclosure.
Claim 3
Dependent Claim
13 words
The process of claim 1, wherein the starter rod is comprised of silicon.
Claim 4
Dependent Claim
15 words
The process of claim 1, wherein the starter rod is a single crystal silicon rod.
Claim 5
Dependent Claim
17 words
The process of claim 1, wherein the starter rod has a diameter of less than 2 cm.
Claim 6
Dependent Claim
17 words
The process of claim 2, wherein the starter rod has a diameter of less than 1 cm.
Claim 7
Dependent Claim
23 words
The process of claim 1, wherein substantially all of the powder from the effluent is removed prior to being recycled to the enclosure.
Claim 8
Dependent Claim
23 words
The process of claim 1, wherein the effluent is cooled to a temperature less than 300° C. before being recycled to the enclosure.
Claim 9
Dependent Claim
29 words
The process of claim 1, wherein the effluent is cooled to a temperature in the range from about 50° to about 300° C. before being recycled to the enclosure.
Claim 10
Dependent Claim
29 words
The process of claim 8, wherein the effluent is cooled to a temperature in the range from about 50° to about 100° C. before being recycled to the enclosure.
Claim 11
Dependent Claim
35 words
The process of claim 1, wherein substantially all of the powder from the effluent is removed and the effluent is cooled to temperature of less than 300° C., prior to being recycled to the enclosure.
Claim 12
Dependent Claim
20 words
The process of claim 1, wherein the effective radius of the enclosure is from about 6 to about 15 cm.
Claim 13
Dependent Claim
19 words
The process of claim 1, wherein the starter rod is energized by passing an electric current through the rod.
Claim 14
Dependent Claim
25 words
The process of claim 1, wherein the silane concentration in the cooled enclosure is in the range of from about 0.5 to 10 mole percent.
Claim 15
Dependent Claim
25 words
The process of claim 13, wherein the silane concentration in the cooled enclosure is in the range of from about 1.5 to 5.0 mole percent.
Claim 16
Dependent Claim
52 words
The process of claim 1, wherein the portion of effluent is recycled into the enclosure at a rate sufficient to entrain at least about 25 percent of the silicon powder being formed within the enclosure and removing said powder from the enclosure through the outlet of the enclosure with the exiting effluent.
Claim 17
Dependent Claim
52 words
The process of claim 1, wherein the portion of effluent is recycled into the enclosure at a rate sufficient to entrain at least about 50 percent of the silicon powder being formed within the enclosure and removing said powder from the enclosure through the outlet of the enclosure with the exiting effluent.
Claim 18
Dependent Claim
52 words
The process of claim 1, wherein the portion of effluent is recycled into the enclosure at a rate sufficient to entrain at least about 75 percent of the silicon powder being formed within the enclosure and removing said powder from the enclosure through the outlet of the enclosure with the exiting effluent.
Claim 19
Dependent Claim
20 words
The process of claim 1, wherein the effluent is recycled at a rate of at least 2.5×10 5 cubic cm./min.
Claim 20
Dependent Claim
24 words
The process of claim 1, wherein the effluent is recycled at a rate of at about 5×10 4 to about 15×10 6 cubic cm./min.
Claim 21
Dependent Claim
23 words
The process of claim 1, wherein the effluent is recycled at a rate sufficient to decrease the thickness of the thermal boundary layer.
Claim 22
Dependent Claim
33 words
The process of claim 1, wherein the effluent is recycled at a rate sufficient to provide uniform temperature within the thermal boundary a layer substantially along the entire axial length of the rod.
Claim 23
Dependent Claim
25 words
The process of claim 1, wherein the effluent is recycled at a rate greater than 20 m 3 /hr per 1 kg/hr of silicon production.
Claim 24
Dependent Claim
27 words
The process of claim 22, wherein the effluent is recycled at a rater greater than 20 to 2,000 m 3 /hr per 1 kg/hr of silicon production.
Claim 25
Dependent Claim
23 words
The process of claim 1, wherein the bulk temperature of the effluent leaving the enclosure through the outlet is less than 400° C.
Claim 26
Dependent Claim
23 words
The process of claim 24, wherein the bulk temperature of the effluent leaving the enclosure through the outlet is less than 300° C.
Claim 27
Dependent Claim
19 words
The process of claim 1, wherein the enclosure is at atmospheric pressure up to 10 bars of absolute pressure.
Claim 28
Dependent Claim
15 words
The process of claim 1, wherein the final rod diameter is at least 8 cm.
Claim 29
Dependent Claim
15 words
The process of claim 1, wherein the final rod diameter is at least 10 cm.
Claim 30
Dependent Claim
15 words
The process of claim 1, wherein the final rod diameter is at least 12 cm.
Claim 31
Dependent Claim
40 words
The process of claim 1, wherein the recycled effluent enters the lower inlet of the enclosure in a manner such that the effluent flows upwardly in a uniform and circumferential manner along and around the length of the silicon rod.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1992-05-01 | 1992-10-31 | 1993-05-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1996-05-01 | 1996-10-31 | 1997-05-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2000-05-01 | 2000-10-31 | 2001-05-02 | $7700.00 | Window Closed / Lapsed |