EP0881987A1 - Silice pure fondue, four et procede de production - Google Patents

Silice pure fondue, four et procede de production

Info

Publication number
EP0881987A1
EP0881987A1 EP97905726A EP97905726A EP0881987A1 EP 0881987 A1 EP0881987 A1 EP 0881987A1 EP 97905726 A EP97905726 A EP 97905726A EP 97905726 A EP97905726 A EP 97905726A EP 0881987 A1 EP0881987 A1 EP 0881987A1
Authority
EP
European Patent Office
Prior art keywords
refractory
accordance
fumace
halogen
fused silica
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
EP97905726A
Other languages
German (de)
English (en)
Other versions
EP0881987A4 (fr
Inventor
Robert S. Pavlik, Jr.
Daniel R. Sempolinski
Michael H. Wasilewski
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Corning Inc
Original Assignee
Corning Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Corning Inc filed Critical Corning Inc
Publication of EP0881987A1 publication Critical patent/EP0881987A1/fr
Publication of EP0881987A4 publication Critical patent/EP0881987A4/fr
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1407—Deposition reactors therefor
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1484—Means for supporting, rotating or translating the article being formed
    • C03B19/1492—Deposition substrates, e.g. targets
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/02—Pure silica glass, e.g. pure fused quartz
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/02—Pure silica glass, e.g. pure fused quartz
    • C03B2201/03—Impurity concentration specified
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/50—Multiple burner arrangements
    • C03B2207/52—Linear array of like burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/50—Multiple burner arrangements
    • C03B2207/54—Multiple burner arrangements combined with means for heating the deposit, e.g. non-deposition burner

Definitions

  • An article of relatively pure fused silica and a furnace and method for producing the article.
  • Relatively pure metal oxides are produced by thermal decomposition of precursors and deposition ofthe resulting oxides.
  • the precursor may take the form of a vapor, or may be carried by a vapor. It may be decomposed by either flame hydrolysis or pyrolysis.
  • One such process is production of fused silica by hydrolysis or pyrolysis of silicon tetrachloride.
  • Early patents disclosing such processes for producing silica are United States Patent No. 2,239,551 (Nordberg) and 2,272,342 (Hyde).
  • a commercial application of flame hydrolysis involves forming and depositing particles of fused silica to form large bodies (boules). Such boules may be used individually, or may be finished and integrated together into large optical bodies, such as telescope mirrors.
  • SiCl 4 is hydrolyzed, and the hydrolyzed vapor is passed into a flame to form molten particles of fused silica.
  • the particles are continuously deposited on a bait, or in a crucible, known as a cup, to form a boule.
  • these measures constituted providing a purer zircon refractory for use in constructing a furnace in which the fused silica was deposited to form a boule.
  • dispersants, binders and water relatively free of sodium ions in producing zircon refractory components for the fumace.
  • UV wavelength radiation from an excimer type laser This laser emits radiation at about 193 nm and 248 nm wavelengths.
  • One aspect ofthe present invention resides in an improved method of producing a fused silica body by introducing a silicon-containing compound into a flame to form molten silica particles and collecting those particles in the form of a fused silica body in a fumace constructed of refractory materials, the improvement comprising constructing at least a portion ofthe furnace from refractory materials that have been exposed to a reactive, halogen-containing gas to react with and thereby cleanse the refractory of contaminating metals.
  • a further aspect ofthe invention resides in a relatively pure fused silica material in which the fused silica has a transmittance value of at least 99.5% for 248 nm radiation, a transmittance value of at least 98% for 193 nm radiation, at least a substantial portion of the body has an acceptable fluorescence level when exposed to such radiation, and the fused silica material has a content of contaminating metal ions less than 100 ppb.
  • the invention further resides in a refractory fumace for collecting molten silica particles in the form of a solid body, at least a portion ofthe fumace being constructed of a refractory that contains metal contaminants in an amount less than 300 ppm.
  • FIGURE in the accompanying drawing is a schematic representation of an apparatus and process for depositing a large body of fused silica.
  • the conventional boule process used in making fused silica is a one-step process.
  • a carrier gas is bubbled through a SiCl 4 feedstock that is maintained at a specified low temperature.
  • the vaporous SiCl 4 is entrained in the carrier gas and is thereby transported to the reaction site.
  • the reaction site is comprised of a number of burners that combust and oxidize the vaporous SiCl 4 to deposit silica at a temperature greater than 1600° C.
  • the apparatus and transfer system be capable of vaporizing the feedstock and delivering the vaporized feedstock to a burner in the vapor state.
  • the apparatus and process may remain substantially unchanged with one major exception.
  • the SiCl 4 feedstock is replaced by a polymethylsiloxane.
  • Use of this substitute feedstock may require some minor adjustments, such as a somewhat higher delivery temperature (e.g., 100-150° C). This is due to the siloxane having a somewhat lower vapor pressure than SiCl 4 .
  • FIGURE 1 in the accompanying drawing is a schematic representation of an apparatus and process for producing and depositing molten silica particles to build up a large, fused silica boule.
  • the apparatus generally designated by the numeral 10, includes a feedstock source 12. Nitrogen, or a nitrogen/oxygen mixture, is used as the carrier gas.
  • a bypass stream of nitrogen 14 is introduced to prevent saturation ofthe vaporous stream.
  • the vaporous reactant is passed through a distribution mechamsm to the reaction site wherein a number of burners 18 are present in close proximity to a furnace crown 20.
  • the reactant is combined with a fuel oxygen mixture 22 at these burners, and is combusted and oxidized to deposit silica at a temperature greater than 1 00° C.
  • High purity metal oxide soot and heat are directed downwardly through the refractory fumace crown 20.
  • the silica is immediately deposited and consolidated to a non-porous mass 24 on hot cup 26.
  • Contaminating metals can be present in the raw materials employed in production of fumace refractories.
  • the metals may also be entrained during sintering ofthe refractory, or during any subsequent operations, such as sawing or grinding.
  • Zircon is a relatively clean refractory, particularly when prepared as described in the Sempoiinski et al. patents.
  • the superior transmission properties required for such demanding uses as microlithography applications require control of all metal contaminants at a level below 100 parts per billion (ppb).
  • this degree of contaminating metal control in a collection fumace can be achieved by constructing the furnace of refractory materials containing less than 300 parts per million (ppm) ofthe contaminating metals.
  • ppm parts per million
  • zircon refractories used in a collection furnace for fused silica deposition This desirable end is accomplished, in accordance with the present invention, by firing the fumace refractories in a halogen-containing atmosphere. The halogen reacts with and removes the contaminating metals from at least the exposed surface ofthe refractory.
  • the cleansing gas can be used in essentially pure form. However, we have found it convenient, and effective, to employ as little as 5% ofthe cleansing gas in an inert gas, such as helium or argon, with a somewhat longer treatment time.
  • the cleansing treatment may employ a continuous flow ofthe halogen gas. Alternatively, a pulsed type treatment may be used wherein gas is repeatedly introduced into the firing chamber and subsequently exhausted.
  • the cleansing action can occur at a temperature as low as 700°C. However, it is usually preferred to employ somewhat higher temperatures in the range of 1100 to 1500°C. Above 1500°C, zircon starts to thermally dissociate, thereby resulting in a weaker refractory body.
  • the invention is here described with reference to treatment of zircon refractory fumace elements. However, it will be appreciated that it is also applicable to cleansing contaminating metals from other types of refractory articles.
  • the cleansing process on a refractory body may be carried out either prior to assembly into a fumace or after assembly.
  • the treatment may also be carried out during production ofthe refractory.
  • High temperature refractories, such as zircon are sintered in air at temperatures in excess of 1500°C. As the sintered furnace components are being cooled, the cooling step can be interrupted at an appropriate temperature, for example, 1200°C.
  • the sintering fumace is then switched to a halogen-containing atmosphere, and the temperature maintained for the necessary time to cleanse the refractory ofthe contaminating metals.
  • the use of refractories chemically cleaned in accordance with the invention provides several advantages.
  • the cleaner deposition fumace provides a fused silica product of high purity. It provides high, consistent yields of fused silica glass having an acceptably high transmission of short wavelength UV radiation and a low level of fluorescence. Further, the glass is less prone to increases in radiation damage and fluorescence in service. These desired ends are achieved without requiring change in, or compromise of, either the fumace design or the silica forming and deposition process.
  • the effectiveness ofthe cleansing treatment was demonstrated by comparing two sets of fused silica test pieces. One set was taken from boules deposited in an untreated collection fumace. A second set was taken from boules deposited in a treated fumace.
  • the fiirnaces were constructed in essentially identical design with sintered zircon refractory crowns and cup liners.
  • the refractories in the treated fumace were soaked for eight hours in a furnace operating at 1300°C. A flowing atmosphere of 5.7% Cl 2 and
  • the fused silica boules described above were also analyzed to determine the percentage of boule depth that exhibited an acceptable low level of fluorescence.
  • Fluorescence is determined by integrating the intensities measured over the range of 400- 700 nm. To be acceptable, a glass test piece must exhibit a value, as so determined, that is below 4.2x10' 9 watts/cm 2 when the glass is exposed to an emitting laser operating at 15 mj/cm 2 and 200 Hz. Glass from the untreated fumace was completely unacceptable. There was no portion ofthe boule in which the fluorescence value was acceptably low. Glass from the treated fumace had acceptable glass to a depth of 3.53 inches. This represented 59.3% of the total depth.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Structural Engineering (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Glass Compositions (AREA)

Abstract

Article en silice relativement pure, et four et procédé de production de cet article. Cet article est obtenu par collecte de particules (24) de silice fondues dans un four réfractaire dans lequel au moins une partie du réfractaire a été exposé à un gaz contenant un halogène pour réagir avec les ions métalliques polluants qu'il contient.
EP97905726A 1996-02-21 1997-02-11 Silice pure fondue, four et procede de production Ceased EP0881987A4 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US1199796P 1996-02-21 1996-02-21
US11997P 1996-02-21
PCT/US1997/001681 WO1997030933A1 (fr) 1996-02-21 1997-02-11 Silice pure fondue, four et procede de production

Publications (2)

Publication Number Publication Date
EP0881987A1 true EP0881987A1 (fr) 1998-12-09
EP0881987A4 EP0881987A4 (fr) 1999-05-12

Family

ID=21752895

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97905726A Ceased EP0881987A4 (fr) 1996-02-21 1997-02-11 Silice pure fondue, four et procede de production

Country Status (3)

Country Link
EP (1) EP0881987A4 (fr)
JP (1) JP2000505036A (fr)
WO (1) WO1997030933A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100574123B1 (ko) * 1997-09-24 2006-04-25 코닝 인코포레이티드 용융 실리카-티타니아 유리의 제조방법
US6410192B1 (en) 1999-11-15 2002-06-25 Corning Incorporated Photolithography method, photolithography mask blanks, and method of making
JP2001342026A (ja) * 2000-05-30 2001-12-11 Tosoh Quartz Corp 石英ガラスの製造方法及び製造装置
WO2002049978A1 (fr) 2000-12-21 2002-06-27 Corning Incorporated Refractaires pour fours de production de silice fondue
US9403689B2 (en) 2010-12-02 2016-08-02 Saint-Gobain Ceramics & Plastics, Inc. Zircon components
TWI689475B (zh) * 2015-06-10 2020-04-01 美商康寧公司 從玻璃移除金屬沉積物的方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA936790A (en) * 1971-03-31 1973-11-13 J. Kriegler Rudolph Sio2 structure having resistance to mobile ion contaminates and method for obtaining same
US5395413A (en) * 1993-04-16 1995-03-07 Corning Incorporated Method for producing fused silica with low sodium ion contamination level

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2272342A (en) * 1934-08-27 1942-02-10 Corning Glass Works Method of making a transparent article of silica
US2239551A (en) * 1939-04-22 1941-04-22 Corning Glass Works Method of making sealing glasses and seals for quartz lamps
JPS54134721A (en) * 1978-04-11 1979-10-19 Nippon Telegraph & Telephone Manufacture of anhydrous glass parent material for optical fiber
JPS54160414A (en) * 1978-06-08 1979-12-19 Nippon Telegraph & Telephone Production of optical communication fiber material
JPS6046940A (ja) * 1983-08-22 1985-03-14 Furukawa Electric Co Ltd:The 光学系ガラス母材の製造方法とその装置
DE3836934A1 (de) * 1988-10-29 1990-05-03 Heraeus Schott Quarzschmelze Verfahren zum reinigen von teilchenfoermigem siliziumdioxid
US5043002A (en) * 1990-08-16 1991-08-27 Corning Incorporated Method of making fused silica by decomposing siloxanes

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA936790A (en) * 1971-03-31 1973-11-13 J. Kriegler Rudolph Sio2 structure having resistance to mobile ion contaminates and method for obtaining same
US5395413A (en) * 1993-04-16 1995-03-07 Corning Incorporated Method for producing fused silica with low sodium ion contamination level

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO9730933A1 *

Also Published As

Publication number Publication date
JP2000505036A (ja) 2000-04-25
WO1997030933A1 (fr) 1997-08-28
EP0881987A4 (fr) 1999-05-12

Similar Documents

Publication Publication Date Title
US5523266A (en) Optical member of synthetic quartz glass for excimer lasers and method for producing same
CA2056271C (fr) Verre permeable aux uv et articles comportant ce verre
EP0737654B2 (fr) Méthode de production de silice fondue de grande pureté ayant une haute résistance aux dommages optiques, et silice fondue de grande pureté
JP5403853B2 (ja) 高透過率合成シリカガラスおよびその製造方法
KR0130007B1 (ko) 유리질실리카제품 및 그 제조방법
US5332702A (en) Low sodium zircon refractory and fused silica process
US6174509B1 (en) Pure fused silica, furnace and method
JP2004203736A (ja) 高純度溶融シリカの製造方法
US6619073B2 (en) Method of increasing the initial transmittance of optical glass
JP2006516525A (ja) 合成シリカガラスの製造方法
WO1997030933A1 (fr) Silice pure fondue, four et procede de production
US6574991B1 (en) Pure fused silica, furnace and method
US6630418B2 (en) Fused silica containing aluminum
EP1456142B1 (fr) Silice fondue contenant de l'aluminium
WO2001017919A1 (fr) Silice pure fondue, four et procede correspondants
JPH1053432A (ja) 石英ガラス光学部材、その製造方法、及び投影露光装置
US6763683B2 (en) Method for pure, fused oxide
US20030205057A1 (en) Method and apparatus for adding metals to fused silica
US20040250572A1 (en) Method for producing radiation-resistant quartz glass material, and quartz glass material
JPS58151341A (ja) 光伝送用ガラスフアイバ−の製法

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19980902

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): DE FR GB NL

RIN1 Information on inventor provided before grant (corrected)

Inventor name: WASILEWSKI, MICHAEL, H.

Inventor name: SEMPOLINSKI, DANIEL, R.

Inventor name: PAVLIK, ROBERT, S., JR.

A4 Supplementary search report drawn up and despatched

Effective date: 19990330

AK Designated contracting states

Kind code of ref document: A4

Designated state(s): DE FR GB NL

RA4 Supplementary search report drawn up and despatched (corrected)

Effective date: 19990415

17Q First examination report despatched

Effective date: 20000114

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION HAS BEEN REFUSED

18R Application refused

Effective date: 20050509