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US4444811A Expired / Lapsed US ⏱️ 0.0 years remaining

Fluidized bed silicon deposition from silane

Assignee: California Institute of Technology
•
Filing: 1981-12-03
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Granted: 1984-04-24
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Expires: 2001-12-03
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Abstract

Abstract A process and apparatus for thermally decomposing silicon containing gas for deposition on fluidized nucleating silicon seed particles is disclosed. Silicon seed particles are produced in a secondary fluidized reactor by thermal decomposition of a silicon containing gas. The thermally produced silicon seed particles are then introduced into a primary fluidized bed reactor to form a fludized bed. Silicon containing gas is introduced into the primary reactor where it is thermally decomposed and deposited on the fluidized silicon seed particles. Silicon seed particles having the desired amount of thermally decomposed silicon product thereon are removed from the primary fluidized reactor as ultra pure silicon product. An apparatus for carrying out this process is also disclosed.

Inventors

  • 👤 George Hsu
  • 👤 Harry Levin
  • 👤 Richard A. Hogle
  • 👤 Ananda Praturi
  • 👤 Ralph Lutwack

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 05:15
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/44; C23C16/442; C01; C01B; C01B33/00; C01B33/02; C01B33/021; C01B33/027; C01B33/029; C01B33/03

Claims Analysis

Total Claims: 22
Claim 1
Independent Claim 356 words
A process for producing silicon comprising the steps of: introducing fluidizing gas into a primary fluidized reactor zone in an amount sufficient to maintain a bed of silicon seed particles in a fluidized introducing a silicon containing gas capable of gas phase thermal decomposition into said primary fluidized reactor zone; heating said primary fluidized reactor zone to a temperature sufficient to thermally decompose the silicon in said silicon containing gas to elemental silicon but not above the melting point temperature of silicon; depositing the elemental silicon formed by said thermally decomposed silicon containing gas on said suspended seed particles; continuously removing said seed particles with elemental silicon deposited thereon from said primary fluidized reactor as silicon product; removing excess fluidizing gas, unreacted silicon containing gas, reaction by-product gases and any entrained silicon particles therein from said primary fluidized reactor zone; continuously reintroducing silicon seed particles into said primary fluidized reactor zone to replace silicon seed particles which are removed as silicon product; and producing a continuous supply of said silicon seed particles for introduction into said primary fluidized reactor zone by thermally decomposing a seed generating gas containing silicon in a pyrolysis seed reactor zone to form precursor seed particles including the steps of; introducing said seed generating gas into said seed reactor zone; heating said pyrolysis seed reactor to a temperature sufficient to thermally decompose the silicon in said seed generating gas to form elemental silicon, but not above the melting point temperature of silicon; passing a protective inert gas inwardly through porous reactor walls to form a protective inert gas boundary to prevent contact of silicon with the porous reactor walls; thermally decomposing the silicon in said seed generating gas to form precursor silicon seed particles; removing said precursor silicon seed particles from said pyrolysis seed reactor zone; separating said precursor silicon seed particles into larger silicon seed particles for introducing into said primary fluidged reactor zone and smaller silicon particles which are recycled back to said pyrolysis seed reactor zone for further growth and introducing said separated larger precursor silicon seed particles into said primary fluidized reactor zone as the silicon seed particles.
Claim 2
Dependent Claim 356 words
A process for producing silicon comprising the steps of: introducing fluidizing gas into a primary fluidized reactor zone in an amount sufficient to maintain a bed of silicon seed particles in a fluidized introducing a silicon containing gas capable of gas phase thermal decomposition into said primary fluidized reactor zone; heating said primary fluidized reactor zone to a temperature sufficient to thermally decompose the silicon in said silicon containing gas to elemental silicon but not above the melting point temperature of silicon; depositing the elemental silicon formed by said thermally decomposed silicon containing gas on said suspended seed particles; continuously removing said seed particles with elemental silicon deposited thereon from said primary fluidized reactor as silicon product; removing excess fluidizing gas, unreacted silicon containing gas, reaction by-product gases and any entrained silicon particles therein from said primary fluidized reactor zone; continuously reintroducing silicon seed particles into said primary fluidized reactor zone to replace silicon seed particles which are removed as silicon product; and producing a continuous supply of said silicon seed particles for introduction into said primary fluidized reactor zone by thermally decomposing a seed generating gas containing silicon in a pyrolysis seed reactor zone to form precursor seed particles including the steps of; introducing said seed generating gas into said seed reactor zone; heating said pyrolysis seed reactor to a temperature sufficient to thermally decompose the silicon in said seed generating gas to form elemental silicon, but not above the melting point temperature of silicon; passing a protective inert gas inwardly through porous reactor walls to form a protective inert gas boundary to prevent contact of silicon with the porous reactor walls; thermally decomposing the silicon in said seed generating gas to form precursor silicon seed particles; removing said precursor silicon seed particles from said pyrolysis seed reactor zone; separating said precursor silicon seed particles into larger silicon seed particles for introducing into said primary fluidged reactor zone and smaller silicon particles which are recycled back to said pyrolysis seed reactor zone for further growth and introducing said separated larger precursor silicon seed particles into said primary fluidized reactor zone as the silicon seed particles.
Claim 3
Dependent Claim 32 words
The process of claim 1 wherein said precursor silicon seed particles are separated into seed particles having diameters substantially greater than 50 microns and recycle particles having diameters less than 50 microns.
Claim 4
Dependent Claim 171 words
The process of claim 1 which further includes the steps of: introducing said precursor silicon seed particles into a secondary fluidized reactor zone; introducing fluidizing gas into said second fluidized reactor zone in an amount sufficient to maintain said precursor silicon seed particles in fluidized suspension; introducing a silicon containing gas capable of gas phase thermal decomposition into said secondary fluidized reactor zone; heating said secondary fluidized reactor zone to a temperature sufficient to thermally decompose the silicon in said silicon containing gas to elemental silicon, but not above the melting point temperature of silicon; depositing the elemental silicon formed by said thermally decomposed silicon containing gas on said suspended precursor seed particles; continuously removing said precursor silicon seed particles with elemental silicon deposited thereon from said secondary fluidized reactor zone and transporting them to said primary fluidized reactor zone for introduction as said silicon seed particles; and removing excess fluidizing gas, unreacted silicon containing gas, reaction by-product gases and any entrained silicon particles therein from said secondary fluidized reactor zone.
Claim 5
Dependent Claim 44 words
The process of claim 3 which further includes the step of separating said entrained silicon particles from said excess fluidizing gas, unreacted silicon containing gas and reaction by-product gases and recycling said separated out entrained silicon particles back into said secondary fluidized reactor zone.
Claim 6
Dependent Claim 25 words
The process of claim 1 wherein said precursor silicon seed particles removed from said pyrolysis seed reactor zone have diameters between 0.1 and 5 microns.
Claim 7
Dependent Claim 62 words
The process of claim 1 wherein the heating of said pyrolyzer seed reactor zone is provided by a heating element disposed internally within said pyrolysis seed reactor zone wherein silicon is prevented from contacting said heating element by passing an inert gas outwardly through a porous layer encompassing said heating element to provide a protective inert gas boundary surrounding said heating element.
Claim 8
Dependent Claim 46 words
The process of claim 6 which additionally includes the step of separating said precursor silicon seed particles into silicon seed particles for introduction into said primary fluidized reactor zone and smaller silicon particles which are recycled back to said pyrolysis seed reactor zone for further growth.
Claim 9
Dependent Claim 170 words
The process of claim 6 which additionally includes the steps of: introducing said precursor silicon seed particles into a secondary fluidized reactor zone; introducing fluidizing gas into said second fluidized reactor zone in an amount sufficient to maintain said precursor silicon seed particles in fluidized suspension; introducing a silicon containing gas capable of gas phase thermal decomposition into said second fluidized reactor zone; heating said second fluidized reactor zone to a temperature sufficient to thermally decompose the silicon in said silicon containing gas to elemental silicon, but not above the melting point temperature of silicon; depositing the elemental formed by said thermally decomposed silicon containing gas on said suspended precursor seed particles; continuously removing said precursor silicon seed particles with elemental silicon deposited thereon from said secondary fluidized reactor zone and transporting them to said primary fluidized reactor zone for introduction as said silicon seed particles; and removing excess fluidizing gas, unreacted silicon containing gas, reaction by-product gases and any entrained silicon particles therein from said secondary fluidized reactor zone.
Claim 10
Dependent Claim 40 words
The process of claim 1 wherein the entrained particles removed from said primary fluidized reactor zone are separated from the excess fluidizing gas, unreacted silicon containing gas and reaction by-product gases and reintroduced back into said primary fluidized reactor zone.
Claim 11
Dependent Claim 23 words
The process of claim 1 wherein the fluidizing gas is introduced into said primary fluidized reactor zone through a plurality of gas inlets.
Claim 12
Dependent Claim 25 words
The process of claim 1 wherein said fluidizing gas and said gas containing silicon are mixed prior to introduction into said primary fluidized reactor zone.
Claim 13
Dependent Claim 25 words
The process of claim 3 wherein said fluidizing gas and said gas containing silicon are mixed prior to entry into said secondary fluidized reactor zone.
Claim 14
Dependent Claim 28 words
The process of claim 11 wherein said fluidizing gas being introduced into said primary fluidized reactor zone contains between about 5% and 100% by volume silicon containing gas.
Claim 15
Dependent Claim 28 words
The process of claim 12 wherein said fluidizing gas being introduced into said secondary fluidized reactor zone contains between about 5% and 100% by volume silicon containing gas.
Claim 16
Dependent Claim 13 words
The process according to claim 1 wherein said silicon containing gas is silane.
Claim 17
Dependent Claim 25 words
The process according to claim 1 wherein said seed generating gas contains from between about 5% to 100% by volume of a silicon containing gas.
Claim 18
Dependent Claim 13 words
The process according to claim 1 wherein said silicon containing gas is silane.
Claim 19
Dependent Claim 20 words
The process of claim 1 wherein said primary fluidized reactor zone is heated to between about 400° to 1200° C.
Claim 20
Dependent Claim 23 words
The process of claim 1 wherein said pyrolysis seed reactor zone is heated to a temperature of between about 400° and 1200° C.
Claim 21
Dependent Claim 23 words
The process of claim 3 wherein said secondary fluidized reactor zone is heated to a temperature of between about 400° and 1200° C.
Claim 22
Dependent Claim 25 words
A process according to claim 13 in which the seed reactor zone is heated by a heating element disposed centrally and axially in said zone.

References Cited (Backward Citations)

CA613772A Cited
US2915367A Cited
US4207360A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1987-04-24 1987-10-24 1988-04-24 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1991-04-24 1991-10-24 1992-04-24 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1995-04-24 1995-10-24 1996-04-24 $7700.00 Window Closed / Lapsed

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