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US5154744A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of making titania-doped fused silica

Assignee: Corning Inc
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Filing: 1991-08-26
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Granted: 1992-10-13
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Expires: 2011-08-26
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Abstract

Abstract This invention relates to production of high purity fused silica glass doped with titania through oxidation or flame hydrolysis of a gaseous mixture and containing rutile crystals comprising a vaporizable, silicon-containing compound. Titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, constitute the operable titanium-containing compounds.

Inventors

  • 👤 Jeffery L. Blackwell
  • 👤 Carlton M. Truesdale

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 13:13
CPC Classifications
C; C03; C03B; C03B37/00; C03B37/01; C03B37/012; C03B37/014; C03B37/01413; C03C; C03C1/00; C03C3/00; C03C3/04; C03C3/06; C03B2201/00; C03B2201/06; C03B2201/30; C03B2201/40; C03B2201/42; C03B2207/00; C03B2207/30; C03B2207/32; C03B2207/80; C03B2207/81; C03B2207/85; C03B2207/87; C03C2201/00; C03C2201/06; C03C2201/30; C03C2201/40; C03C2201/42; C03C2203/00; C03C2203/40; Y; Y02; Y02P; Y02P40/00; Y02P40/50; Y02P40/57; Y10; Y10S; Y10S65/00; Y10S65/901

Claims Analysis

Total Claims: 18
Claim 1
Independent Claim 187 words
In a method for making a non-porous body of high purity fused silica glass doped with titania comprising the steps of: (a) producing a gas stream containing a silicon-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to SiO 2 and a titanium-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to TiO 2; (b) passing said gas stream into the flame of a combustion burner to form amorphous particles of fused SiO 2 doped with TiO 2 and containing submicroscopic crystals of rutile and anatase with rutile being the predominant crystal phase; (c) depositing said amorphous particles onto a support; and (d) either essentially simultaneously with said deposition or subsequently thereto consolidating said deposit of amorphous particles into a non-porous body; the improvement comprising utilizing as said titanium-containing compound in vapor form a halide-free, titanium-containing compound selected from the group consisting of titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, whereby no halide-containing vapors are emitted from said titanium-containing compound during the making of said porous body.
Claim 2
Dependent Claim 187 words
In a method for making a non-porous body of high purity fused silica glass doped with titania comprising the steps of: (a) producing a gas stream containing a silicon-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to SiO 2 and a titanium-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to TiO 2; (b) passing said gas stream into the flame of a combustion burner to form amorphous particles of fused SiO 2 doped with TiO 2 and containing submicroscopic crystals of rutile and anatase with rutile being the predominant crystal phase; (c) depositing said amorphous particles onto a support; and (d) either essentially simultaneously with said deposition or subsequently thereto consolidating said deposit of amorphous particles into a non-porous body; the improvement comprising utilizing as said titanium-containing compound in vapor form a halide-free, titanium-containing compound selected from the group consisting of titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, whereby no halide-containing vapors are emitted from said titanium-containing compound during the making of said porous body.
Claim 3
Dependent Claim 13 words
A method according to claim 1 wherein said silicon-containing compound is also halide-free.
Claim 4
Dependent Claim 14 words
A method according to claim 2 wherein said halide-free, silicon-containing compound is a polymethylcyclosiloxane.
Claim 5
Dependent Claim 11 words
A method according to claim 3 wherein said polymethylcyclosiloxane is octamethylcyclosiloxane.
Claim 6
Dependent Claim 17 words
A method according to claim 1 wherein said gas stream is comprised of natural gas and oxygen.
Claim 7
Dependent Claim 188 words
In a method for making optical waveguide fibers of high purity fused silica glass doped with titania comprising the steps of: (a) producing a gas stream containing a silicon-containing compound in vapor form capable of being converted through heat treatment with oxidation or flame hydrolysis to SiO 2 and a titanium-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to TiO 2; (b) passing said gas stream into the flame of a combustion burner to form amorphous particles of fused SiO 2 doped with TiO 2 and containing submicroscopic crystals of rutile and anatase with rutile being the predominant crystal phase; (c) depositing said amorphous particles onto a mandrel; (d) consolidating said deposit of amorphous particles into a non-porous, transparent glass body; and (e) drawing waveguide fiber from said body; the improvement comprising utilizing as said titanium-containing compound in vapor form a halide-free, titanium-containing compound selected from the group consisting of titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, whereby no halide-containing vapors are emitted from said titania-containing compound during the making of said optical waveguide fibers.
Claim 8
Dependent Claim 188 words
In a method for making optical waveguide fibers of high purity fused silica glass doped with titania comprising the steps of: (a) producing a gas stream containing a silicon-containing compound in vapor form capable of being converted through heat treatment with oxidation or flame hydrolysis to SiO 2 and a titanium-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to TiO 2; (b) passing said gas stream into the flame of a combustion burner to form amorphous particles of fused SiO 2 doped with TiO 2 and containing submicroscopic crystals of rutile and anatase with rutile being the predominant crystal phase; (c) depositing said amorphous particles onto a mandrel; (d) consolidating said deposit of amorphous particles into a non-porous, transparent glass body; and (e) drawing waveguide fiber from said body; the improvement comprising utilizing as said titanium-containing compound in vapor form a halide-free, titanium-containing compound selected from the group consisting of titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, whereby no halide-containing vapors are emitted from said titania-containing compound during the making of said optical waveguide fibers.
Claim 9
Dependent Claim 13 words
A method according to claim 6 wherein said silicon-containing compound is also halide-free.
Claim 10
Dependent Claim 14 words
A method according to claim 7 wherein said halide-free, silicon-containing compound is a polymethylcyclosiloxane
Claim 11
Dependent Claim 11 words
A method according to claim 8 wherein said polymethylcyclosiloxane is octamethylcyclosiloxane.
Claim 12
Dependent Claim 17 words
A method according to claim 6 wherein said gas stream is comprised of natural gas and oxygen.
Claim 13
Dependent Claim 189 words
In a method for making optical waveguide fibers of high purity fused silica glass doped with titania comprising steps of: (a) producing a gas stream containing a silicon-containing compound in vapor form capable of being converted through heat treatment with oxidation or flame hydrolysis to SiO 2 and a titanium-containing compound in vapor form capable of being converted through thermal decomposition with oxidation of flame hydrolysis to TiO 2; (b) passing said gas stream into a flame of a combustion burner to form amorphous particles of fused SiO 2 doped with TiO 2 and containing submicroscopic crystals of rutile and anatase with rutile being the redominant crystal phase; (c) depositing said amorphous particles onto the surface of a bait tube; (d) consolidating said amorphous particles into a non-porous, transparent glass body; and (e) drawing waveguide fiber from said body; the improvement comprising utilizing as said titanium-containing compound in vapor form a halide-free, titanium-containing compound selected from the group consisting of titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, whereby no halide-containing vapors are emitted from said titanium-containing compound during the making of said optical waveguide fibers.
Claim 14
Dependent Claim 189 words
In a method for making optical waveguide fibers of high purity fused silica glass doped with titania comprising steps of: (a) producing a gas stream containing a silicon-containing compound in vapor form capable of being converted through heat treatment with oxidation or flame hydrolysis to SiO 2 and a titanium-containing compound in vapor form capable of being converted through thermal decomposition with oxidation of flame hydrolysis to TiO 2; (b) passing said gas stream into a flame of a combustion burner to form amorphous particles of fused SiO 2 doped with TiO 2 and containing submicroscopic crystals of rutile and anatase with rutile being the redominant crystal phase; (c) depositing said amorphous particles onto the surface of a bait tube; (d) consolidating said amorphous particles into a non-porous, transparent glass body; and (e) drawing waveguide fiber from said body; the improvement comprising utilizing as said titanium-containing compound in vapor form a halide-free, titanium-containing compound selected from the group consisting of titanium-2-ethylhexyloxide, titanium cyclopentyloxide, and a titanium amide, or a combination thereof, whereby no halide-containing vapors are emitted from said titanium-containing compound during the making of said optical waveguide fibers.
Claim 15
Dependent Claim 13 words
A method according to claim 11 wherein said silicon-containing compound is also halide-free.
Claim 16
Dependent Claim 14 words
A method according to claim 12 wherein said halide-free, silicon-containing compound is a polymethylcyclosiloxane.
Claim 17
Dependent Claim 11 words
A method according to claim 13 wherein said polymethylcyclosiloxane is octamethylcyclosilane.
Claim 18
Dependent Claim 14 words
A method according to claim 11 wherein said gas stream is comprised of oxygen.

References Cited (Backward Citations)

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JPS56114904A Cited
JPS56164023A Cited
US4501602A Cited
JPS6090838A Cited
US4768859A Cited
US4877306A Cited
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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) 1995-10-13 1996-04-13 1996-10-13 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1999-10-13 2000-04-13 2000-10-13 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2003-10-13 2004-04-13 2004-10-13 $7700.00 Window Closed / Lapsed

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