WO2004083144A1 - High homogeneity silica glass prepared through a sol-gel procedure - Google Patents

High homogeneity silica glass prepared through a sol-gel procedure Download PDF

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Publication number
WO2004083144A1
WO2004083144A1 PCT/EP2004/002577 EP2004002577W WO2004083144A1 WO 2004083144 A1 WO2004083144 A1 WO 2004083144A1 EP 2004002577 W EP2004002577 W EP 2004002577W WO 2004083144 A1 WO2004083144 A1 WO 2004083144A1
Authority
WO
WIPO (PCT)
Prior art keywords
sol
silica glass
wave length
internal transmittance
gel
Prior art date
Application number
PCT/EP2004/002577
Other languages
French (fr)
Inventor
Fulvio Costa
Lorenzo Costa
Massimo Sparpaglione
Original Assignee
Degussa Novara Technology S.P.A.
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 Degussa Novara Technology S.P.A. filed Critical Degussa Novara Technology S.P.A.
Priority to BRPI0408614-7A priority Critical patent/BRPI0408614A/en
Priority to EP04719938A priority patent/EP1603842A1/en
Priority to AU2004222147A priority patent/AU2004222147A1/en
Priority to JP2006500059A priority patent/JP2006520735A/en
Priority to CA002519666A priority patent/CA2519666A1/en
Priority to US10/549,680 priority patent/US20060079387A1/en
Publication of WO2004083144A1 publication Critical patent/WO2004083144A1/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
    • 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
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
    • 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
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/02—Pure silica glass, e.g. pure fused quartz
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/26—Wet processes, e.g. sol-gel process using alkoxides

Definitions

  • the present invention relates to a highly homogeneous Si0 glass prepared through a sol-gel procedure.
  • the sol-gel terra defines a wide variety of processes which, even if being different as for as the working details or the reagents are concerned, are characterized by the following common operations :
  • X generally is an alcohol residue and n means the element M valence;
  • the alcoxydes M(OR)n can be replaced by soluble salts of the element M such as chlorides or nitrates, and, in some cases, oxyides.
  • sol a solution or a colloidal suspension
  • the solvent is removed through a simple controlled evaporation, which determines the so called xerogel, or through an extraction in autoclave which determines the so called aerogel;
  • the obtained body is a porous glass, which may have an apparent density of 10% to about 50% of the theoric density of the oxide having the same composition; the dried gel can be industrially used as such;
  • the final densification let a glassy product be obtained having good general characteristics, and, however, without any such optical homogeneity property to let the material be crossed by the transmitted light wave front without any suffered distortion.
  • the object of the present invention is a silica glass characterized, inter alia, by the following specific properties :
  • such a silica glass being prepared according to a sol-gel process wherein, in the meanwhile the densification is achieved, a treatment is carried out by means of an atmosphere containing water traces.

Landscapes

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

Abstract

The present invention relates to a Si2O glass characterized by a high homogeneity, prepared through a sol-gel procedure.

Description

HIGH HOMOGENEITY SILICA GLASS PREPARED THROUGH A SOL-GEL PROCEDURE
The present invention relates to a highly homogeneous Si0 glass prepared through a sol-gel procedure.
The sol-gel terra defines a wide variety of processes which, even if being different as for as the working details or the reagents are concerned, are characterized by the following common operations :
- preparation of a solution, or a suspension, of a precursor formed by a compound of the element (M) the oxide of which has to constitute the final glassy article;
- hydrolysis, acid or base catalyzed, of the precursor, inside the solution or suspension, to form M-OH groups according to the reaction
MXn + nH20 → M(OH)n + nHX
wherein X generally is an alcohol residue and n means the element M valence; the alcoxydes M(OR)n can be replaced by soluble salts of the element M such as chlorides or nitrates, and, in some cases, oxyides. The obtained mixture, i.e. a solution or a colloidal suspension, is named sol;
- polycondensation of the M-OH groups according to the reaction
M-OH + M-OH → M-O-M + H20
which requires a time from few seconds to some days, depending on the solution composition and the temperature; during this step, a matrix is formed called, case by case, alcohogel, hydrogel or more generally, gel;
- gel drying till the formation of a porous monolithic body; during this step, the solvent is removed through a simple controlled evaporation, which determines the so called xerogel, or through an extraction in autoclave which determines the so called aerogel; the obtained body is a porous glass, which may have an apparent density of 10% to about 50% of the theoric density of the oxide having the same composition; the dried gel can be industrially used as such;
- densification of the dried gel by a treatment at a temperature, generally ranging between 800°C and 1500°C, depending on the gel chemical composition and the preceding step process parameters; during this step the porous gel is becoming dense, under a controlled atmosphere, till to obtain a glassy or ceramic compact oxide having the theoric density, with a linear shrinkage equal to about 50%.
The final densification let a glassy product be obtained having good general characteristics, and, however, without any such optical homogeneity property to let the material be crossed by the transmitted light wave front without any suffered distortion.
The Applicant has found that in the case suitable treatments under controlled atmosphere are carried out during the densification stage, the final glassy product is obtained having no streak and strip, the same being consequently characterized by an almost total homogeneity. Therefore, the object of the present invention is a silica glass characterized, inter alia, by the following specific properties :
light internal transmittance in the wave length between 185nm and 193nm higher than 85%
light internal transmittance in the wave length between 193nm and 2600nm higher than 99.5%
light internal transmittance in the wave length between 2600nm and 273Onm higher than 99%
- light internal transmittance in the wave length between 2730nm and 3200nm higher than 85%
- no streak, material of class 4 or better according to the rule DIN ISO 10110-4
- no strip
- no signal in the shadography (no shadow or intensity change)
such a silica glass being prepared according to a sol-gel process wherein, in the meanwhile the densification is achieved, a treatment is carried out by means of an atmosphere containing water traces.

Claims

Claims
1. Silica glass characterized by the following specific properties:
- light internal transmittance in the wave length between 185nm and 193nm higher than 85%
light internal transmittance in the wave length between 193nm and 2600nm higher than 99.5%
light internal transmittance in the wave length between 2600nm and 273On higher than 99%
light internal transmittance in the wave length between 273Onm and 3200nm higher than 85%
- no streak, material of class 4 or better according to the rule DIN ISO 10110-4
- no strip
- no signal in the shadography (no shadow or intensity change)
such a silica glass being prepared according to a sol- gel process wherein, in the meanwhile the densification is achieved, a treatment is carried out by means of an atmosphere containing water traces .
PCT/EP2004/002577 2003-03-21 2004-03-12 High homogeneity silica glass prepared through a sol-gel procedure WO2004083144A1 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
BRPI0408614-7A BRPI0408614A (en) 2003-03-21 2004-03-12 high homogeneity silica glass prepared by a sol-gel procedure
EP04719938A EP1603842A1 (en) 2003-03-21 2004-03-12 High homogeneity silica glass prepared through a sol-gel procedure
AU2004222147A AU2004222147A1 (en) 2003-03-21 2004-03-12 High homogeneity silica glass prepared through a sol-gel procedure
JP2006500059A JP2006520735A (en) 2003-03-21 2004-03-12 High homogeneity silica glass produced by the sol-gel method
CA002519666A CA2519666A1 (en) 2003-03-21 2004-03-12 High homogeneity silica glass prepared through a sol-gel procedure
US10/549,680 US20060079387A1 (en) 2003-03-21 2004-03-12 High homogeneity silica glass prepared through a sol-gel procedure

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITNO2003A000005 2003-03-21
IT000005A ITNO20030005A1 (en) 2003-03-21 2003-03-21 HIGH HOMOGENEITY SiO2 GLASSES.

Publications (1)

Publication Number Publication Date
WO2004083144A1 true WO2004083144A1 (en) 2004-09-30

Family

ID=33017984

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2004/002577 WO2004083144A1 (en) 2003-03-21 2004-03-12 High homogeneity silica glass prepared through a sol-gel procedure

Country Status (11)

Country Link
US (1) US20060079387A1 (en)
EP (1) EP1603842A1 (en)
JP (1) JP2006520735A (en)
KR (1) KR100814627B1 (en)
CN (1) CN1761630A (en)
AU (1) AU2004222147A1 (en)
BR (1) BRPI0408614A (en)
CA (1) CA2519666A1 (en)
IT (1) ITNO20030005A1 (en)
RU (1) RU2005132393A (en)
WO (1) WO2004083144A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2174916A1 (en) * 2008-10-09 2010-04-14 Universite Des Sciences Et Technologies De Lille Highly pure silica monoliths and method of synthesizing same

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9249028B2 (en) 2010-02-08 2016-02-02 Momentive Performance Materials Inc. Method for making high purity metal oxide particles and materials made thereof
US8197782B2 (en) * 2010-02-08 2012-06-12 Momentive Performance Materials Method for making high purity metal oxide particles and materials made thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4681615A (en) * 1982-12-23 1987-07-21 Seiko Epson Kabushiki Kaisha Silica glass formation process
EP0310486A2 (en) * 1987-09-30 1989-04-05 Shin-Etsu Chemical Co., Ltd. A method for the preparation of silica glass
US5063179A (en) * 1990-03-02 1991-11-05 Cabot Corporation Process for making non-porous micron-sized high purity silica
US5068208A (en) * 1991-04-05 1991-11-26 The University Of Rochester Sol-gel method for making gradient index optical elements
US6360564B1 (en) * 2000-01-20 2002-03-26 Corning Incorporated Sol-gel method of preparing powder for use in forming glass

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITNO990004A1 (en) * 1999-03-08 2000-09-08 Gel Design And Engineering S R SOL-GEL PROCESS FOR THE PRODUCTION OF CONTAINING AND ADERENTIAD ARTICLES AND AN INCOMPRESSABLE CYLINDRICAL INSERT AND MANUFACTURES SO OBTAINED.
US6467312B1 (en) * 2000-07-11 2002-10-22 Fitel Usa Corp. Sol gel method of making an optical fiber with multiple apetures

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4681615A (en) * 1982-12-23 1987-07-21 Seiko Epson Kabushiki Kaisha Silica glass formation process
EP0310486A2 (en) * 1987-09-30 1989-04-05 Shin-Etsu Chemical Co., Ltd. A method for the preparation of silica glass
US5063179A (en) * 1990-03-02 1991-11-05 Cabot Corporation Process for making non-porous micron-sized high purity silica
US5068208A (en) * 1991-04-05 1991-11-26 The University Of Rochester Sol-gel method for making gradient index optical elements
US6360564B1 (en) * 2000-01-20 2002-03-26 Corning Incorporated Sol-gel method of preparing powder for use in forming glass

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
TSENG T Y ET AL: "Various atmosphere effects on sintering of compacts of SiO/sub 2/ microspheres", J. MATER. SCI. (UK), JOURNAL OF MATERIALS SCIENCE, OCT. 1986, UK, vol. 21, no. 10, 1986, pages 3615 - 3624, XP001189680, ISSN: 0022-2461 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2174916A1 (en) * 2008-10-09 2010-04-14 Universite Des Sciences Et Technologies De Lille Highly pure silica monoliths and method of synthesizing same
WO2010040910A1 (en) * 2008-10-09 2010-04-15 Universite Des Sciences Et Technologies De Lille High-purity silica monoliths and process for the synthesis thereof
US8563620B2 (en) 2008-10-09 2013-10-22 Universite Des Sciences Et Technologies De Lille High purity silica monoliths and process for the synthesis thereof

Also Published As

Publication number Publication date
ITNO20030005A1 (en) 2004-09-22
AU2004222147A1 (en) 2004-09-30
CA2519666A1 (en) 2004-09-30
US20060079387A1 (en) 2006-04-13
CN1761630A (en) 2006-04-19
EP1603842A1 (en) 2005-12-14
KR100814627B1 (en) 2008-03-18
BRPI0408614A (en) 2006-03-07
KR20050113241A (en) 2005-12-01
JP2006520735A (en) 2006-09-14
RU2005132393A (en) 2006-06-10

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