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US4172883A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of purifying metallurgical grade silicon employing reduced presure atmospheric control

Assignee: National Aeronautics and Space Administration
•
Filing: 1978-06-23
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Granted: 1979-10-30
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Expires: 1998-06-23
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Abstract

Abstract A method wherein a quartz tube is charged with chunks of metallurgical grade silicon and/or a mixture of such chunks and high purity quartz sand, and impurities from a class including aluminum, boron, and the like, as well as certain transition metals including nickel, iron, manganese and the like. The tube is then evacuated and heated to a temperature within a range of 800° C. to 1400° C., whereupon a stream of gas comprising a reactant, such as silicon tetrafluoride, continuously is delivered at low pressures through the charge for causing a metathetical reaction of impurities of the silicon and the reactant to occur for forming a volatile halide and leaving a residue of silicon of an improved purity. Additionally, the reactant may include carbon monoxide gas, whereby impurites such as iron and nickel react therewith to form volatile carbonyls.

Inventors

  • 👤 with respect to an invention by Frosch Robert A. Administrator of the National Aeronautics and Space Administration
  • 👤 William M. Ingle
  • 👤 Stephen W. Thompson
  • 👤 Robert E. Chaney

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-01 07:33
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/02; C01B33/037

Claims Analysis

Total Claims: 5
Claim 1
Independent Claim 133 words
In a method of purifying metallurgical grade silicon, the steps comprising: A. charging a quartz tube with chunks of metallurgical grade silicon containing impurities consisting essentially of aluminum and boron; B. heating the silicon to a temperature within a range of 800° C. to 1350° C. in vacuo; C. continuously passing through said chunks a stream of reactant gas at 0.1 torr to one atmosphere consisting essentially of silicon tetrafluoride to effect a metathetical reaction of aluminum and boron impurities of the silicon with the silicon tetrafluoride with AlF 3 and BF 3 being formed and leaving a residue of silicon of improved impurity; and wherein the AlF 3 formed reacts with the surface of the quartz tube to form silicon tetrafluoride and aluminum oxide which deposits as a coating on said surface.
Claim 2
Dependent Claim 133 words
In a method of purifying metallurgical grade silicon, the steps comprising: A. charging a quartz tube with chunks of metallurgical grade silicon containing impurities consisting essentially of aluminum and boron; B. heating the silicon to a temperature within a range of 800° C. to 1350° C. in vacuo; C. continuously passing through said chunks a stream of reactant gas at 0.1 torr to one atmosphere consisting essentially of silicon tetrafluoride to effect a metathetical reaction of aluminum and boron impurities of the silicon with the silicon tetrafluoride with AlF 3 and BF 3 being formed and leaving a residue of silicon of improved impurity; and wherein the AlF 3 formed reacts with the surface of the quartz tube to form silicon tetrafluoride and aluminum oxide which deposits as a coating on said surface.
Claim 3
Dependent Claim 35 words
The method of claim 1 wherein the chunks are of a size within a range of 0.1-10 mm, and the reactant gas is passed through said chunks for a period of four to twenty hours.
Claim 4
Dependent Claim 24 words
The method of claim 2 wherein the quartz tube is characterized by an inside diameter of 1-4 inches and a length of 24-36 inches.
Claim 5
Dependent Claim 34 words
The method of claim 2 wherein the impurities further contain nickel and the reactant gas further contains carbon monoxide and wherein the carbon monoxide reacts with the nickel to form volatile Ni(CO) 4 .

References Cited (Backward Citations)

CA625027A Cited
US1103747A Cited
US2989376A Cited
DE1039752B Cited
US3097068A Cited
US3034886A Cited
US4045541A Cited
US4070444A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1982-10-29 1983-04-30 1983-10-30 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1986-10-29 1987-04-30 1987-10-30 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1990-10-29 1991-04-30 1991-10-30 $7700.00 Window Closed / Lapsed

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