WO2014208523A1 - Verre exempt d'alcali - Google Patents

Verre exempt d'alcali Download PDF

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Publication number
WO2014208523A1
WO2014208523A1 PCT/JP2014/066626 JP2014066626W WO2014208523A1 WO 2014208523 A1 WO2014208523 A1 WO 2014208523A1 JP 2014066626 W JP2014066626 W JP 2014066626W WO 2014208523 A1 WO2014208523 A1 WO 2014208523A1
Authority
WO
WIPO (PCT)
Prior art keywords
less
glass
compaction
alkali
mgo
Prior art date
Application number
PCT/JP2014/066626
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English (en)
Japanese (ja)
Inventor
周平 野村
和孝 小野
順 秋山
Original Assignee
旭硝子株式会社
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 旭硝子株式会社 filed Critical 旭硝子株式会社
Priority to CN201480036107.XA priority Critical patent/CN105324342B/zh
Priority to CN201910222449.5A priority patent/CN109987836B/zh
Priority to KR1020157036189A priority patent/KR102229428B1/ko
Publication of WO2014208523A1 publication Critical patent/WO2014208523A1/fr

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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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • 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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium

Definitions

  • the present invention is suitable for display substrate glass and photomask substrate glass used in the manufacture of various flat panel displays (FPDs), is substantially free of alkali metal oxides, has low compaction, and can be float-molded. , Relating to alkali-free glass.
  • FPDs flat panel displays
  • Patent Document 1 Conventionally, various display substrate glasses, particularly those in which a metal or oxide thin film is formed on the surface, have been required to have the following characteristics as shown in Patent Document 1, for example. (1) When an alkali metal oxide is contained, alkali metal ions diffuse into the thin film and deteriorate the film characteristics, so that the alkali metal ions are not substantially contained. (2) Sufficient chemical durability against various chemicals used for semiconductor formation.
  • buffered hydrofluoric acid (BHF: mixture of hydrofluoric acid and ammonium fluoride) for etching SiO x and SiN x , and chemicals containing hydrochloric acid used for etching ITO, various acids used for etching metal electrodes (Nitric acid, sulfuric acid, etc.) Resistant to alkali of resist stripping solution. (3) There are no defects (bubbles, striae, inclusions, pits, scratches, etc.) inside and on the surface.
  • BHF mixture of hydrofluoric acid and ammonium fluoride
  • a-Si amorphous silicon
  • p-Si polycrystalline silicon
  • a glass having a small average thermal expansion coefficient is required to increase productivity and thermal shock resistance by increasing the temperature raising / lowering rate of the heat treatment during liquid crystal display production.
  • glass compaction is required to be low in order to minimize dimensional changes associated with glass deformation and glass structural stability when exposed to high temperatures in the thin film formation process. It has been.
  • An object of the present invention is to provide an alkali-free glass having a low compaction, a small average thermal expansion coefficient, and easy float forming.
  • the compaction C1 is 5 ppm or less
  • the compaction C2 is 40 ppm or less
  • expressed in mass% based on the oxide SiO 2 64 to 72, Al 2 O 3 17-22, MgO 1-8, CaO 4 to 15.5, And an alkali-free glass satisfying 0.20 ⁇ MgO / (MgO + CaO) ⁇ 0.41.
  • the compaction C1 is 5 ppm or less
  • the compaction C2 is 25 ppm or less
  • expressed in mass% based on the oxide, SiO 2 67.5-72, Al 2 O 3 17-21, MgO 1-6, CaO 4 to 8.5, Containing SiO 2 , Al 2 O 3 , MgO and CaO are 96% by mass or more in total, It is preferable that 0.22 ⁇ MgO / (MgO + CaO) ⁇ 0.39.
  • the compaction C1 is 5 ppm or less
  • the compaction C2 is 40 ppm or less
  • expressed in mass% based on the oxide, SiO 2 64 to 68, Al 2 O 3 17-22, MgO 2.3-8, CaO 9 to 15.5, Containing SiO 2 , Al 2 O 3 , MgO and CaO are 96% by mass or more in total, It is preferable that 0.22 ⁇ MgO / (MgO + CaO) ⁇ 0.39.
  • the alkali-free glass of the present invention is suitable as a substrate glass for various displays and a substrate glass for a photomask, but can also be used as a glass substrate for a magnetic disk.
  • glass substrates for various displays and photomasks that are required to minimize deformation due to glass deformation and glass structural stabilization when exposed to high temperatures in the thin film formation process. It is effective as a glass substrate.
  • the composition range of each component will be described. If SiO 2 exceeds 72% (mass%, the same unless otherwise specified), the devitrification temperature T L may increase. In addition, the viscosity is increased, and there is a risk that bubbles may be mixed in due to an increase in melting temperature or bubbles that cannot be completely removed during clarification. If it is less than 64%, the ratio of network formers decreases, and compaction increases. Moreover, an average thermal expansion coefficient becomes large. In the first aspect of the alkali-free glass of the present invention, SiO 2 content is less 72% or more 67.5%.
  • the viscosity will be high, the melting temperature will increase, and bubbles may not be removed at the time of clarification, and bubbles may be mixed in. If it is less than 67.5%, compaction may increase. 68% or more is more preferable.
  • the SiO 2 content is 64% or more and 68% or less. If it exceeds 68%, the melting temperature may increase. 67% or less is more preferable. If it is less than 64%, compaction may increase. Moreover, an average thermal expansion coefficient becomes large.
  • the devitrification temperature T L may increase. Further, since it works as a network former like SiO 2, if it exceeds 22%, the viscosity increases, and there is a possibility that the melting temperature rises and bubbles are mixed. If it is less than 17%, the compaction will increase.
  • the Al 2 O 3 content is 17% or more and 21% or less. If it exceeds 21%, the devitrification temperature T L may increase. 20.5% or less is more preferable. If it is less than 17%, the compaction will increase. 18% or more is more preferable.
  • the Al 2 O 3 content is 17% or more and 22% or less. If it exceeds 22%, the devitrification temperature T L may increase. 21% or less is more preferable. If it is less than 17%, the compaction will increase. 18% or more is more preferable.
  • the glass transition point Tg decreases.
  • compaction increases and the average coefficient of thermal expansion increases. If it is less than 1%, the solubility will deteriorate, the Young's modulus will decrease, and the devitrification temperature TL will increase.
  • the MgO content is 1% or more and 6% or less. If it exceeds 6%, the glass transition point Tg decreases, the compaction increases, and the average thermal expansion coefficient increases. 5% or less is more preferable. If it is less than 1%, the devitrification temperature TL will increase. In addition, Young's modulus decreases. 2% or more is more preferable.
  • the MgO content is 2.3% or more and 8% or less. If it exceeds 8%, compaction increases and the average thermal expansion coefficient becomes large. If it is less than 2.3%, the devitrification temperature T L will increase. In addition, Young's modulus decreases. 4% or more is more preferable.
  • the CaO content is 4% or more and 8.5% or less. If it exceeds 8.5%, the compaction will increase and the devitrification temperature TL will increase. If it is less than 4%, the solubility deteriorates, the melting temperature rises, and the devitrification temperature also rises. 5% or more is more preferable.
  • the CaO content is 9% or more and 15.5% or less. If it exceeds 15.5%, the compaction will increase and the devitrification temperature TL will increase. If it is less than 9%, the solubility deteriorates and the dissolution temperature rises. 10% or more is more preferable.
  • MgO / (CaO + MgO) is higher than 0.41, compaction at the time of heat treatment at 600 ° C. increases. Moreover, an average thermal expansion coefficient becomes large. 0.39 or less is preferable and 0.37 or less is more preferable. When it is lower than 0.20, the devitrification temperature T L increases. 0.22 or more is preferable and 0.24 or more is more preferable.
  • the other components are preferably less than 5%, more preferably less than 4%, more preferably less than 3%, even more preferably less than 1%, and still more preferably in order to achieve both high Young's modulus and low compaction. Is less than 0.5%, and particularly preferably, it is substantially not contained, that is, excluding inevitable impurities. Accordingly, in the present invention, the total content of SiO 2 , Al 2 O 3 , CaO, and MgO is preferably 95% or more, more preferably 96% or more, and 97% or more. More preferably, it is 99% or more, more preferably 99.5% or more. It is particularly preferred that it consists essentially of SiO 2 , Al 2 O 3 , CaO and MgO, excluding unavoidable impurities.
  • the B 2 O 3 can be contained to improve the melting reactivity of the glass. However, if the amount is too large, the Young's modulus decreases and the compaction increases. Therefore, the content is preferably less than 3%, more preferably less than 1%, and particularly preferably not contained.
  • BaO can be included to improve the solubility of the glass.
  • the content is preferably less than 5%, more preferably less than 3%, even more preferably less than 1%, even more preferably less than 0.5%, substantially It is particularly preferable that it is not contained in.
  • the SrO can be contained to improve solubility. However, if the amount is too large, the average thermal expansion coefficient increases, so the content is preferably less than 5%.
  • the SrO content is preferably less than 3%, more preferably less than 1%, even more preferably less than 0.5%, and substantially no content. Particularly preferred.
  • the content of SrO is preferably less than 2%, more preferably less than 1%, more preferably less than 0.3%, and particularly preferably not contained.
  • ZrO 2 can be contained to improve the Young's modulus of the glass. However, if the amount is too large, the devitrification temperature increases, so the content is preferably less than 3%, more preferably less than 1%, and particularly preferably not contained.
  • the total amount of ZnO, SO 3 , Fe 2 O 3 , F, Cl and SnO 2 is less than 1%, preferably 0.8%. It can be contained less than 5%, more preferably less than 0.3%, and even more preferably less than 0.1%.
  • the glass of the present invention does not contain an alkali metal oxide in excess of the impurity level (ie substantially) in order not to cause deterioration of the characteristics of the metal or oxide thin film provided on the glass surface during panel production.
  • PbO, As 2 O 3 and Sb 2 O 3 are not substantially contained.
  • the alkali-free glass of the present invention has a very low compaction.
  • Compaction is the glass heat shrinkage generated by relaxation of the glass structure during the heat treatment.
  • compaction means a value measured by the method described below.
  • the target glass is melted at 1550 ° C. to 1650 ° C., then the molten glass is poured out, formed into a plate shape, and then cooled.
  • the obtained plate glass is polished to obtain a glass plate of 100 mm ⁇ 20 mm ⁇ 1 mm.
  • the obtained glass plate is heated to the glass transition point Tg + 70 ° C., held at this temperature for 1 minute, and then cooled to room temperature at a temperature drop rate of 40 ° C./min.
  • the alkali-free glass of the present invention has a compaction C1 of 5 ppm or less.
  • the compaction C2 is 40 ppm or less.
  • the alkali-free glass of the present invention has a compact film C1, C2 satisfying the above conditions, and therefore, when exposed to high temperatures in a thin film forming process performed in the process of manufacturing various displays using the alkali-free glass, The dimensional change accompanying the deformation of the glass and the stabilization of the glass structure can be minimized.
  • compaction C1 is 5 ppm or less.
  • the compaction C2 is 25 ppm or less, and more preferably 20 ppm or less.
  • the compaction C1 is 5 ppm or less.
  • compaction C2 is 40 ppm or less, and 35 ppm or less is more preferable.
  • the alkali-free glass of the present invention has a temperature T 2 at which the viscosity ⁇ becomes 10 2 poise (dPa ⁇ s) in order to facilitate melting and to suppress erosion of the refractory bricks constituting the melting furnace. It is preferable that it is 1760 degrees C or less. In the first aspect of the alkali-free glass of the present invention, it is preferred that T 2 is 1760 ° C. or less. 1740 ° C. is more preferable, and 1720 ° C. or lower is even more preferable. In the second embodiment of the alkali-free glass of the present invention, T 2 is preferably 1730 ° C. or lower. 1710 degrees C or less is more preferable, and 1690 degrees C or less is still more preferable.
  • the alkali-free glass of the present invention preferably has a temperature T 4 at which the viscosity ⁇ becomes 10 4 poise (dPa ⁇ s) of 1380 ° C. or lower in order to facilitate float forming.
  • T 4 is 1380 ° C. or less. 1360 ° C. is more preferable, and 1340 ° C. or less is even more preferable.
  • T 4 is preferably 1360 ° C. or lower. 1340 degrees C or less is more preferable, and 1320 degrees C or less is still more preferable.
  • the alkali-free glass of the present invention has an average thermal expansion coefficient of 40 ⁇ 10 ⁇ 7 / ° C. or less at 50 to 350 ° C. in order to increase the thermal shock resistance and increase the productivity during panel manufacture.
  • the average thermal expansion coefficient at 50 to 350 ° C. is preferably 37 ⁇ 10 ⁇ 7 / ° C. or less, more preferably 34 ⁇ 10 ⁇ 7 / ° C. or less. preferable.
  • the average thermal expansion coefficient at 50 to 350 ° C. is preferably 40 ⁇ 10 ⁇ 7 / ° C. or less, and more preferably 38 ⁇ 10 ⁇ 7 / ° C. or less.
  • the alkali-free glass of the present invention has a glass transition point of 780 ° C. or higher in order to suppress thermal shrinkage during panel production and to make it possible to apply a method by laser annealing as a method for producing p-Si TFTs. Is preferred.
  • the glass transition point is 780 ° C. or more, the fictive temperature of the glass tends to increase in the production process (for example, organic EL having a thickness of 0.7 mm or less, preferably 0.5 mm or less, more preferably 0.3 mm or less) Suitable for a display substrate or lighting substrate for use in the like, or a thin display substrate or lighting substrate having a thickness of 0.3 mm or less, preferably 0.1 mm or less.
  • the alkali-free glass of the present invention can be produced, for example, by the following method.
  • the raw materials of each component that are normally used are blended so as to become target components, which are continuously charged into a melting furnace, heated to 1550 to 1650 ° C. and melted.
  • the molten glass is formed into a predetermined plate thickness by the float method, and then the glass plate can be obtained by slow cooling and cutting.
  • examples 1 to 12 are examples, and examples 13 to 15 are comparative examples.
  • the raw materials of each component were prepared so as to have a target composition, and were melted at a temperature of 1550 to 1650 ° C. using a platinum crucible. In melting, the mixture was stirred using a platinum stirrer to homogenize the glass. Next, the molten glass was poured out, formed into a plate shape, and then slowly cooled.
  • the glass composition (unit: mass%), density ⁇ (g / cm 3 ), Young's modulus E (GPa) (measured by ultrasonic method), specific modulus E / ⁇ (GPa ⁇ cm 3 / g), glass transition point Tg (unit: ° C.), average thermal expansion coefficient ⁇ (unit: ⁇ 10 ⁇ 7 / ° C.) at 50 to 350 ° C., temperature T 2 (glass viscosity ⁇ becomes 10 2 poises) (Unit: ° C.), temperature T 4 (unit: ° C.) at which the glass viscosity ⁇ is 10 4 poise, and compaction C1, C2 (measured by the method described above, unit: ppm) are shown.
  • the values shown in parentheses are calculated values.
  • the glass of the example has a compaction C1 of 5 ppm or less and a compaction C2 of 40 ppm or less.
  • the average thermal expansion coefficient at 50 to 350 ° C. is 40 ⁇ 10 ⁇ 7 / ° C. or less.
  • the alkali-free glass of the present invention is suitable as a substrate glass for various displays and a substrate glass for a photomask, but can also be used as a glass substrate for a magnetic disk.
  • glass substrates for various displays and photomasks that are required to minimize deformation due to glass deformation and glass structural stabilization when exposed to high temperatures in the thin film formation process. It is effective as a glass substrate.

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

Abstract

L'invention concerne un verre exempt d'alcali qui présente un faible compactage, un coefficient de dilatation thermique moyen entre 50 et 350°C faible, et un formage par flottage aisé. Plus précisément, l'invention concerne un verre exempt d'alcali dont un compactage (C1) est inférieur ou égal à 5ppm et un compactage (C2) est inférieur ou égal à 40ppm, qui comprend en % massique sur la base des oxydes, 64 à 72 de SiO2, 17 à 22 de Al2O3, 1 à 8 de MgO et 4 à 15,5 de CaO, et tel que 0,20≦MgO/(MgO+CaO)≦0,41.
PCT/JP2014/066626 2013-06-27 2014-06-24 Verre exempt d'alcali WO2014208523A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201480036107.XA CN105324342B (zh) 2013-06-27 2014-06-24 无碱玻璃
CN201910222449.5A CN109987836B (zh) 2013-06-27 2014-06-24 无碱玻璃
KR1020157036189A KR102229428B1 (ko) 2013-06-27 2014-06-24 무알칼리 유리

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013134900A JP2016153345A (ja) 2013-06-27 2013-06-27 無アルカリガラス
JP2013-134900 2013-06-27

Publications (1)

Publication Number Publication Date
WO2014208523A1 true WO2014208523A1 (fr) 2014-12-31

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ID=52141857

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PCT/JP2014/066626 WO2014208523A1 (fr) 2013-06-27 2014-06-24 Verre exempt d'alcali

Country Status (5)

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JP (1) JP2016153345A (fr)
KR (1) KR102229428B1 (fr)
CN (2) CN105324342B (fr)
TW (1) TW201509856A (fr)
WO (1) WO2014208523A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107709258A (zh) * 2015-07-03 2018-02-16 旭硝子株式会社 载体基板、层叠体、电子器件的制造方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018038059A1 (fr) * 2016-08-23 2018-03-01 旭硝子株式会社 Verre non alcalin

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JP2000302475A (ja) * 1999-04-12 2000-10-31 Carl Zeiss:Fa アルカリ非含有アルミノ硼珪酸ガラスとその用途
JP2001348247A (ja) * 2000-05-31 2001-12-18 Asahi Glass Co Ltd 無アルカリガラス
JP2002003240A (ja) * 2000-06-19 2002-01-09 Nippon Electric Glass Co Ltd 液晶ディスプレイ用ガラス基板
JP2005320180A (ja) * 2004-05-06 2005-11-17 Central Glass Co Ltd ガラス板の熱収縮率を低減させる熱処理方法
WO2012137780A1 (fr) * 2011-04-08 2012-10-11 旭硝子株式会社 Verre non alcalin pour substrats et son procédé de fabrication

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JP4737709B2 (ja) * 2004-03-22 2011-08-03 日本電気硝子株式会社 ディスプレイ基板用ガラスの製造方法
CN101331090B (zh) * 2005-12-16 2014-04-16 日本电气硝子株式会社 无碱玻璃基板及其制造方法
CN101370742B (zh) * 2006-01-12 2012-06-13 日本电气硝子株式会社 无碱玻璃基板
WO2009131053A1 (fr) * 2008-04-21 2009-10-29 旭硝子株式会社 Plaque de verre pour panneau d’affichage, son procédé de fabrication et procédé de fabrication d’un panneau tft
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JP2000302475A (ja) * 1999-04-12 2000-10-31 Carl Zeiss:Fa アルカリ非含有アルミノ硼珪酸ガラスとその用途
JP2001348247A (ja) * 2000-05-31 2001-12-18 Asahi Glass Co Ltd 無アルカリガラス
JP2002003240A (ja) * 2000-06-19 2002-01-09 Nippon Electric Glass Co Ltd 液晶ディスプレイ用ガラス基板
JP2005320180A (ja) * 2004-05-06 2005-11-17 Central Glass Co Ltd ガラス板の熱収縮率を低減させる熱処理方法
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107709258A (zh) * 2015-07-03 2018-02-16 旭硝子株式会社 载体基板、层叠体、电子器件的制造方法
US20180122838A1 (en) * 2015-07-03 2018-05-03 Asahi Glass Company, Limited Carrier substrate, laminate, and method for manufacturing electronic device
CN114538771A (zh) * 2015-07-03 2022-05-27 Ａｇｃ株式会社 载体基板、层叠体、电子器件的制造方法
US11587958B2 (en) * 2015-07-03 2023-02-21 AGC Inc. Carrier substrate, laminate, and method for manufacturing electronic device

Also Published As

Publication number Publication date
CN105324342A (zh) 2016-02-10
JP2016153345A (ja) 2016-08-25
CN109987836B (zh) 2022-03-01
TW201509856A (zh) 2015-03-16
KR102229428B1 (ko) 2021-03-18
KR20160023700A (ko) 2016-03-03
CN109987836A (zh) 2019-07-09
CN105324342B (zh) 2019-04-09

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