WO2005099357A1 - Procede permettant la production d'un verre de silice presentant une resistance thermique elevee - Google Patents

Procede permettant la production d'un verre de silice presentant une resistance thermique elevee Download PDF

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Publication number
WO2005099357A1
WO2005099357A1 PCT/KR2004/000844 KR2004000844W WO2005099357A1 WO 2005099357 A1 WO2005099357 A1 WO 2005099357A1 KR 2004000844 W KR2004000844 W KR 2004000844W WO 2005099357 A1 WO2005099357 A1 WO 2005099357A1
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WO
WIPO (PCT)
Prior art keywords
groups
glass
quartz glass
high heat
manufacturing high
Prior art date
Application number
PCT/KR2004/000844
Other languages
English (en)
Inventor
Han-Seog Oh
Shin Kim
Sung-Eun Park
Original Assignee
Sebit Co., Ltd
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 Sebit Co., Ltd filed Critical Sebit Co., Ltd
Priority to PCT/KR2004/000844 priority Critical patent/WO2005099357A1/fr
Publication of WO2005099357A1 publication Critical patent/WO2005099357A1/fr

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
    • C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • 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
    • C03B2201/04—Hydroxyl ion (OH)
    • 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
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
    • C03C2201/23—Doped silica-based glasses containing non-metals other than boron or halide containing hydroxyl groups
    • 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
    • C03C2203/50—After-treatment
    • C03C2203/52—Heat-treatment
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Definitions

  • the present invention relates to a method for manufacturing high heat-resistant quartz glass, which is used for a high temperature poly-Si TFT-LCD (Thin Film Transistor- Liquid Crystal Display) substrate and in a semiconductor process.
  • a high temperature poly-Si TFT-LCD Thin Film Transistor- Liquid Crystal Display
  • soda-lime glass is the most commonly used glass, which is used to a manufacture of window glass or bottle glass.
  • the soda-lime glass is made of a mixture of silicon oxide, calcium oxide and sodium oxide, and such composition is similar to that of the first glass made by human.
  • Soda-lime glass which is also often referred as lime glass for short, covers approximately 90% of the total glass production, since it can be manufactured with the lowest production cost and easily formed to various shapes of glasses. It has good durability to chemicals, however has poor resistance to high temperature and dramatic temperature changes. Lead-alkali glass has relatively higher cost than that of soda lime glass.
  • Borosilicate glass has long been used for the longest time as a glass that has a strong resistance to thermal shock or dramatic temperature changes. With the borosilicate glass, it is possible to work at a high temperature condition compared to soda-lime glass and lead-alkali glass, and it has very good chemical durability, however its production is difficult than those of soda-lime glass and lead-alkali glass.
  • Aluminosilicate glass has a strong resistance to thermal shock, and can stand the higher temperature compared to the temperature at which borosilicate glass resists.
  • its production is far much difficult than that of borosilicate glass.
  • silica glass is referred to a glass manufactured by a proprietary process, and it can stand extreme thermal shock and very high temperature such as 900 ° C, thereby being suitably used as various industrial products such as a suspended window of an electric furnace, a supporting die for drying. Additionally, it is further used as an outer window of a spaceship, since it can resist the heat generated during the approach of a spaceship to the atmosphere layer of the earth. Quartz glass is uniquely comprised of only monoxide unlike other 5 groups of glasses, and particularly composed of amorphous, i.e. non-crystalline silica. When other material is added to the quartz glass, it becomes a different type of glass.
  • Quartz glass is the most expensive one among other glasses, and has the strongest resistance to thermal shock, and the possible highest temperature condition where it can be used is 900 ° C for a long term use and 1200 °C for a short term use.
  • quartz glass is the best, and used to fields where specific requirements are demanded, such as mirror blank of an astronomical telescope, an optical waveguide, a crucible for crystal development and the like.
  • its production is very difficult, and the shape, which can be formed, is also restricted.
  • the process is relatively independent of the temperature, but in case of an LCD, which uses glass as a substrate, the heat resistance of the glass should be primarily concerned, since LCD is sensitive to temperature.
  • Glass used for TFT-LCD should meet the required conditions such as low density, high heat resistance, high durability, chemical resistance, mechanical properties and the like.
  • the heat resistance of quartz glass i.e. the viscosity at high temperature greatly depends on the concentration of OH group contained in the quartz glass in a way that the heat resistance is improved when the concentration of OH group is low.
  • the heat resistance of quartz glass can be evaluated by thermal deformation, thermal shrinkage and the like, which has a close relation with the concentration of OH group.
  • the object of the present invention is to solve the above-mentioned problems in conventional arts and to provide an economic and simple process for removing OH groups contained in porous silica to lower the concentration of OH groups in the quartz glass to lOOppm or less, thereby providing quartz glass with improved heat resistance.
  • the present inventors have found that the concentration of OH groups in glass can be decreased to lOOppm or less, through a rapid heating process under a vacuum condition to remove OH groups contained in porous silica and a transparent glass forming step, and thus completed the present invention which relates to a method for manufacturing quartz glass with improved heat resistance.
  • the present invention relates to a method for manufacturing high heat resistant quartz glass comprising the steps of: a step of removing OH groups where porous silica is rapidly heated to high temperature under a vacuum condition; and a step of forming transparent glass.
  • the present invention relates to a method for manufacturing high heat resistant quartz glass, characterized in that the step of removing OH groups comprises rapid heating to 1000°C ⁇ 1300°C, more preferably to 1200 ° C ⁇ 1300 ° C, under a vacuum condition, at the rate of temperature elevation of 150 ⁇ 250 "C/min to remove OH groups.
  • the rate of the temperature elevation is less than 150 ° C7min, the effect of removing OH groups is lower, and the rate of the temperature elevation of not less than 250 ° C/min is hardly achieved in the current technical state of the art.
  • the glass manufactured according to the present invention is characterized by having the OH concentration of 400ppm or less, and preferably lOOppm or less.
  • the rapid heating process is advantageous in an economic aspect of making the process time shorter to improve productivity, and a technical aspect of increasing the temperature at which porous silica is shrank, thereby removmg OH groups more effectively. If OH groups are not removed before the shrinkage of the porous silica, air bubbles are likely to be remained in the final glass products resulted from the subsequent transparent glass forming process.
  • rapid heating for removing OH groups the temperature is higher than the temperature elevated by a general heating process, and thus the more OH groups can be removed.
  • the heating temperature is excessively high, interparticle agglomeration of porous silica is preceded, and thus gases in the atmosphere become locked in the glass.
  • the heating temperature in the step of removing OH groups is suitably in the range oflOOO °C ⁇ 1300 °C , and preferably in the order of 1200 °C ⁇ 1300 ° C . It is effective that the heating process for removing OH groups is practiced in vacuum condition. In an inert gas atmosphere such as Ar and the like or in the air, OH groups are not sufficiently removed, and further damages may be occurred after the transparent glass forming process, thereby hardly obtaining transparent glass.
  • Example 1 Porous silica was heated in a graphite furnace at the rate of 200 ° C/min, maintained at 1000°C for 10 hours to remove OH groups, heated again at the rate of 10 ° C/min, maintained at 1450 ° C for 1 hour for glass forming and cooled. In the process, the atmosphere was maintained under vacuum of 10 "2 torr. The surface of the resulted glass was polished. By using an infrared spectrometer, the concentration of OH groups was detennined to be 339ppm.
  • Example 2> The same process as in Example 1 was carried out, except that the heated porous silica was maintained for 20 hours in the step of removing OH groups. The resulted concentration of OH groups was 329ppm.
  • Example 3> The same process as in Example 1 was carried out, except that the heated porous silica was maintained for 40 hours in the step of removing OH groups. The resulted concentration of OH groups was 292ppm.
  • Example 4 The same process as in Example 2 was carried out, except that the heating temperature was 1100 ° C in the step of removing OH groups. The resulted concentration of OH groups was 270ppm.
  • Example 5 The same process as in Example 2 was carried out, except that the heating temperature was 1200 °C in the step of removing OH groups. The resulted concentration of OH groups was 59ppm.
  • Example 6 The same process as in Example 2 was carried out, except that the heating temperature was 1300 °C in the step of removing OH groups. The resulted concentration of OH groups was 25ppm.
  • Porous silica was heated in a graphite furnace at the rate of 10 ° C/min, maintained at 1000 °C for 10 hours to remove OH groups, heated again at the rate of 10 ° C/min, maintained at 1450 °C for 1 hour for glass forming and cooled. In the process, the atmosphere was maintained in Ar atmosphere. It was failed to obtain transparent glass, thereby being impossible to determine the concentration of OH groups.
  • Comparative Example 2 The same process as in Comparative Example 1 was carried out, except that the atmosphere during heating was changed to the air. It was failed to obtain transparent glass, thereby being impossible to determine the concentration of OH groups.
  • Comparative Example 3 The same process as in Comparative Example 2 was carried out, except that the heating temperature was changed to 1100 ° C in the step of removing OH groups. It was failed to obtain transparent glass, thereby being impossible to determine the concentration of OH groups.
  • Comparative Example 4 The same process as in Comparative Example 2 was carried out, except that the heating temperature was changed to 1200°C in the step of removing OH groups. It was failed to obtain transparent glass, thereby being impossible to determine the concentration of OH groups.
  • Comparative Example 5 The same process as in Comparative Example 2 was carried out, except that the heating temperature was changed to 1300 ° C in the step of removing OH groups. It was failed to obtain transparent glass, thereby being impossible to determine the concentration of OH groups. Test conditions such as atmosphere during heat treatment, conditions for removing OH groups, conditions for forming transparent glass and the like, and the resulted concentration of OH groups were summarized in Table 1 below.
  • quartz glass which is used for a high temperature Poly-Si TFT-LCD substrate or in a semiconductor process
  • a relatively simple device and process which comprises rapidly heating porous silica under vacuum atmosphere to effectively remove OH groups, and ca ⁇ ying out a transparent glass forming process.
  • the process time is reduced so that the quartz glass can be mass-produced in economic way.
  • the present invention provides high heat-resistant quartz glass being free of the contamination of halogen atoms.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention concerne un procédé permettant la production d'un verre de silice présentant une haute résistance thermique, et plus spécifiquement un procédé permettant de produire un verre de silice présentant une résistance thermique élevée, destiné à la production de substrats TFT LCD Poly-Si, et à la fabrication de semi-conducteurs, ce procédé consistant à éliminer le groupe OH en soumettant la silice à un refroidissement rapide sous vide.
PCT/KR2004/000844 2004-04-13 2004-04-13 Procede permettant la production d'un verre de silice presentant une resistance thermique elevee WO2005099357A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/KR2004/000844 WO2005099357A1 (fr) 2004-04-13 2004-04-13 Procede permettant la production d'un verre de silice presentant une resistance thermique elevee

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/KR2004/000844 WO2005099357A1 (fr) 2004-04-13 2004-04-13 Procede permettant la production d'un verre de silice presentant une resistance thermique elevee

Publications (1)

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WO2005099357A1 true WO2005099357A1 (fr) 2005-10-27

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11162427B2 (en) * 2018-08-06 2021-11-02 Pratt & Whitney Canada Corp. Thermal blanket for gas turbine engine

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6050108A (en) * 1997-09-08 2000-04-18 Sumitomo Electric Industries, Ltd. Method for producing glass preform
JP2000239031A (ja) * 1998-12-25 2000-09-05 Asahi Glass Co Ltd 合成石英ガラスおよびその製造方法
EP1103528A2 (fr) * 1999-11-24 2001-05-30 Heraeus Quarzglas GmbH & Co. KG Corps en verre de quartz pour un élément optique et procédé de sa fabrication
JP2001302274A (ja) * 2000-04-24 2001-10-31 Sumitomo Metal Ind Ltd 紫外線用石英ガラスおよびその製造方法
WO2003091171A2 (fr) * 2002-04-26 2003-11-06 Heraeus Tenevo Ag Procede pour produire un corps en verre de quartz cylindrique a faible teneur en oh

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6050108A (en) * 1997-09-08 2000-04-18 Sumitomo Electric Industries, Ltd. Method for producing glass preform
JP2000239031A (ja) * 1998-12-25 2000-09-05 Asahi Glass Co Ltd 合成石英ガラスおよびその製造方法
EP1103528A2 (fr) * 1999-11-24 2001-05-30 Heraeus Quarzglas GmbH & Co. KG Corps en verre de quartz pour un élément optique et procédé de sa fabrication
JP2001302274A (ja) * 2000-04-24 2001-10-31 Sumitomo Metal Ind Ltd 紫外線用石英ガラスおよびその製造方法
WO2003091171A2 (fr) * 2002-04-26 2003-11-06 Heraeus Tenevo Ag Procede pour produire un corps en verre de quartz cylindrique a faible teneur en oh

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11162427B2 (en) * 2018-08-06 2021-11-02 Pratt & Whitney Canada Corp. Thermal blanket for gas turbine engine

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