CN109987836B - Alkali-free glass - Google Patents

Alkali-free glass Download PDF

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CN109987836B
CN109987836B CN201910222449.5A CN201910222449A CN109987836B CN 109987836 B CN109987836 B CN 109987836B CN 201910222449 A CN201910222449 A CN 201910222449A CN 109987836 B CN109987836 B CN 109987836B
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alkali
less
glass
free glass
mgo
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CN109987836A (en
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野村周平
小野和孝
秋山顺
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AGC Inc
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Asahi Glass Co Ltd
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    • 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

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  • 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

The present invention relates to alkali-free glasses. The invention relates to alkali-free glass which has low shrinkage rate, small average thermal expansion coefficient at 50-350 ℃ and is easy to float. Specifically, the present invention relates to an alkali-free glass having a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 40ppm or less, wherein the alkali-free glass contains SiO in terms of mass% based on oxides2 64～72、Al2O317-22, 1-8 of MgO, 4-15.5 of CaO, and MgO/(MgO + CaO) is not less than 0.20 and not more than 0.41.

Description

Alkali-free glass
The application is a divisional application of Chinese patent application with application date of 2014, 6 and 24 and application number of 201480036107. X.
Technical Field
The present invention relates to an alkali-free glass which is suitable as a substrate glass for displays or a substrate glass for photomasks used for manufacturing various Flat Panel Displays (FPDs), which contains substantially no alkali metal oxide, has a low shrinkage rate, and can be formed by a float process.
Background
Conventionally, various display substrate glasses, particularly display substrate glasses having a metal, oxide thin film or the like formed on the surface thereof, are 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 in the thin film to deteriorate film characteristics, and therefore, it is required that the alkali metal oxide does not substantially contain alkali metal ions.
(2) Has sufficient chemical durability against various chemicals used in semiconductor formation. Especially for SiOxOr SiNxThe buffered hydrofluoric acid (BHF: a mixed solution of hydrofluoric acid and ammonium fluoride) for etching ITO, a chemical solution containing hydrochloric acid for etching ITO, various acids (nitric acid, sulfuric acid, etc.) for etching a metal electrode, and an alkali of a resist stripping solution have durability.
(3) The interior and the surface are free from defects (bubbles, streaks, inclusions, pits, scratches, etc.).
In addition to the above-described requirements, the following situation has been present in recent years.
(4) The display is required to be lightweight, and glass itself is desired to be low-density glass.
(5) The display is required to be lightweight, and thinning of the substrate glass is desired.
(6) In addition to conventional amorphous silicon (a-Si) type liquid crystal displays, polysilicon (p-Si) type liquid crystal displays (a-Si: about 350 ℃ → p-Si: 350 to 550 ℃) having a slightly higher heat treatment temperature were produced.
(7) Glass having a small average thermal expansion coefficient is required for increasing the temperature increase/decrease rate of heat treatment in the production of liquid crystal displays, thereby improving productivity or thermal shock resistance.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open No. 2001-348247
Disclosure of Invention
Problems to be solved by the invention
In addition to the properties described in the background art, in recent years, when exposed to high temperatures in a film forming process, the shrinkage of glass has been required to be low in order to minimize deformation of glass and dimensional change accompanying structural stabilization of glass.
The invention aims to provide alkali-free glass which has low shrinkage rate and small average thermal expansion coefficient and is easy to float.
Means for solving the problems
The present invention provides an alkali-free glass, wherein the alkali-free glass has a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 40ppm or less, and the alkali-free glass contains, in terms of mass% based on oxides:
Figure BDA0002004061460000021
Figure BDA0002004061460000031
0.20≤MgO/(MgO+CaO)≤0.41。
in the alkali-free glass of the present invention, the alkali-free glass preferably has a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 25ppm or less, and contains, in mass% based on oxides:
Figure BDA0002004061460000032
SiO2、Al2O3MgO and CaO in a total amount of 96 mass% or more, and
0.22≤MgO/(MgO+CaO)≤0.39。
in the alkali-free glass of the present invention, the alkali-free glass preferably has a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 40ppm or less, and contains, in mass% based on oxides:
Figure BDA0002004061460000033
SiO2、Al2O3MgO and CaO in a total amount of 96 mass% or more, and
0.22≤MgO/(MgO+CaO)≤0.39。
effects of the invention
The alkali-free glass of the present invention is suitable as substrate glass for various displays or substrate glass for photomasks, and can also be used as a glass substrate for magnetic disks, etc. However, since the shrinkage ratio is low, it is effective as various display substrate glasses or photomask substrate glasses that are required to minimize deformation of glass and dimensional change accompanying structural stabilization of glass when exposed to high temperatures in a film forming process.
Detailed description of the preferred embodiments
Next, the composition ranges of the respective components will be explained. SiO 22When it exceeds 72% (mass%, the same applies hereinafter unless otherwise specified), there is a possibility that the devitrification temperature T will beLAnd (4) rising. Further, the viscosity also increases, and there is a possibility that the melting temperature increases and bubbles are mixed because bubbles are not completely removed at the time of clarification. When the amount is less than 64%, the ratio of network formation decreases and the shrinkage increases. Further, the average thermal expansion coefficient becomes large.
Here, in the alkali-free glass of the invention according to mode 1, SiO2The content is 67.5% or more and 72% or less. If the content exceeds 72%, the viscosity increases, and the melting temperature increases, so that bubbles may not be completely removed during clarification and may be mixed into bubbles. When the amount is less than 67.5%, the shrinkage may increase. More preferably 68% or more.
In mode 2 of the alkali-free glass of the present invention, SiO2The content is 64% or more and 68% or less. If the content exceeds 68%, the melting temperature may be increased. More preferably 67% or less. When the amount is less than 64%, the shrinkage may increase. Further, the average thermal expansion coefficient becomes large.
Al2O3If it exceeds 22%, devitrification temperature T is likely to occurLAnd (4) rising. And, with SiO2Similarly, when the amount of the copolymer is more than 22%, the viscosity increases, and the melting temperature may increase, thereby causing the incorporation of bubbles. When less than 17%, an increase in shrinkage is caused.
Here, in the 1 st aspect of the alkali-free glass of the present invention, Al2O3The content is 17% to 21%. If it exceeds 21%, devitrification temperature T may be reachedLAnd (4) rising. More preferably 20.5% or less. When the amount is less than 17%, the shrinkage rate increases, and more preferably 18% or more.
In mode 2 of the alkali-free glass of the present invention, Al2O3The content is 17% to 22%. If it exceeds 22%, devitrification temperature T is likely to occurLAnd (4) rising. More preferably 21% or less. When the amount is less than 17%, the shrinkage rate increases, and more preferably 18% or more.
When MgO exceeds 8%, the glass transition temperature Tg decreases, the shrinkage increases, and the average coefficient of thermal expansion increases. When the content is less than 1%, the meltability is deteriorated and the Young's modulus is lowered to cause a devitrification temperature TLAnd (4) rising.
Here, the present inventionIn embodiment 1 of the clear alkali-free glass, the MgO content is 1% or more and 6% or less. When the amount exceeds 6%, the glass transition temperature Tg decreases, the shrinkage increases, and the average thermal expansion coefficient increases. More preferably 5% or less. Less than 1%, causes devitrification temperature TLAnd increases and the young's modulus decreases. More preferably 2% or more.
In embodiment 2 of the alkali-free glass of the present invention, the MgO content is 2.3% or more and 8% or less. When the amount exceeds 8%, the shrinkage rate increases and the average thermal expansion coefficient increases. Less than 2.3%, causes devitrification temperature TLAnd (4) rising. Also, the young's modulus decreases. More preferably 4% or more.
When CaO exceeds 15.5%, an increase in shrinkage or devitrification temperature T is causedLIs increased. When the content is less than 4%, the meltability deteriorates, the melting temperature increases, and the devitrification temperature also increases.
In embodiment 1 of the alkali-free glass of the present invention, the CaO content is 4% or more and 8.5% or less. When the amount exceeds 8.5%, an increase in shrinkage or devitrification temperature T is causedLIs increased. When the content is less than 4%, the meltability deteriorates, the melting temperature increases, and the devitrification temperature also increases. More preferably 5% or more.
In embodiment 2 of the alkali-free glass of the present invention, the CaO content is 9% or more and 15.5% or less. When it exceeds 15.5%, an increase in shrinkage or devitrification temperature T is causedLIs increased. When the content is less than 9%, the melting property is deteriorated and the melting temperature is increased. More preferably 10% or more.
When MgO/(CaO + MgO) is more than 0.41, the shrinkage rate in the heat treatment at 600 ℃ increases. Further, the average thermal expansion coefficient becomes large. Preferably 0.39 or less, more preferably 0.37 or less. A devitrification temperature T of less than 0.20LAnd (4) rising. Preferably 0.22 or more, more preferably 0.24 or more.
Other components, for example, the following components may be contained within a range not to impair the effects of the present invention. In this case, the other components are preferably less than 5%, more preferably less than 4%, more preferably less than 3%, still more preferably less than 1%, still more preferably less than 0.5%, particularly preferably substantially not contained,i.e. not containing, apart from unavoidable impurities. Therefore, in the present invention, SiO2、Al2O3The total content of CaO and MgO is preferably 95% or more, more preferably 96% or more, more preferably 97% or more, further preferably 99% or more, and further more preferably 99.5% or more. Particularly preferably substantially consisting of SiO2、Al2O3CaO and MgO, i.e. SiO in addition to unavoidable impurities2、Al2O3CaO and MgO.
B may be contained for improving the melting reactivity of the glass2O3. However, B2O3When too large, the Young's modulus decreases and the shrinkage increases, so that the content is preferably less than 3%, more preferably less than 1%, and particularly preferably substantially not contained.
BaO may be contained to improve the meltability of the glass. However, when BaO is too large, the average thermal expansion coefficient increases, and therefore the content is preferably less than 5%, more preferably less than 3%, still more preferably less than 1%, still more preferably less than 0.5%, and particularly preferably substantially not contained.
SrO may be contained to improve the meltability. However, when SrO is too large, the average thermal expansion coefficient increases, so that the content is preferably less than 5%.
In embodiment 1 of the alkali-free glass of the present invention, the SrO content is preferably less than 3%, more preferably less than 1%, even more preferably less than 0.5%, and particularly preferably substantially none.
In embodiment 2 of the alkali-free glass of the present invention, the SrO content is preferably less than 2%, more preferably less than 1%, even more preferably less than 0.3%, and particularly preferably substantially not contained.
ZrO may be contained for the purpose of enhancing the Young's modulus of the glass2. However, ZrO2If too much, the devitrification temperature is increased, and therefore the content is preferably less than 3%, more preferably less than 1%, and particularly preferably substantially not contained.
In the present invention, the glass raw material may contain less than 1%, preferably less than 1% in total, for the purpose of improving the melting property, the refining property and the formability of the glass0.5%, more preferably less than 0.3%, still more preferably less than 0.1% of ZnO, SO3、Fe2O3、F、Cl、SnO2。
The glass of the present invention does not contain an alkali metal oxide exceeding the impurity level (i.e., does not substantially contain) so as not to cause deterioration in the characteristics of the metal or oxide thin film provided on the glass surface during the production of the panel. Further, in order to facilitate recovery of the glass, it is preferable that PbO and As are not substantially contained2O3、Sb2O3。
The shrinkage rate of the alkali-free glass is extremely low.
The shrinkage rate is a thermal shrinkage rate of glass caused by relaxation of a glass structure during heat treatment. In the present invention, the shrinkage ratio is a value measured by the method described below.
First, a target glass is melted at 1550 to 1650 ℃, then the molten glass is flowed out, formed into a plate shape, cooled, and the obtained plate-shaped glass is polished to obtain a glass plate of 100mm × 20mm × 1 mm.
Next, the resulting glass plate was heated to a glass transition temperature Tg +70 ℃ for 1 minute, and then cooled to room temperature at a cooling rate of 40 ℃/minute. After that, 2 indentations were made on the surface of the glass plate at an interval a (a ═ 90mm) in the longitudinal direction, thereby obtaining a sample before treatment.
Next, the sample before treatment was heated to 450 ℃ at a temperature rising rate of 100 ℃/hr, held at 450 ℃ for 2 hours, and then cooled to room temperature at a temperature lowering rate of 100 ℃/hr, thereby obtaining a sample after treatment 1.
Then, the indentation pitch B1 of the treated sample 1 was measured.
From the thus obtained A, B1, the shrinkage rate C1 was calculated using the following formula.
C1[ppm]＝(A-B1)/A×106
The sample before treatment was heated to 600 ℃ at a temperature rising rate of 100 ℃/hr, held at 600 ℃ for 1 hour, and then cooled to room temperature at a temperature lowering rate of 100 ℃/hr to obtain a sample after treatment 2.
Then, indentation pitch B2 of sample 2 after the treatment was measured.
From the thus obtained A, B2, the shrinkage rate C2 was calculated using the following formula.
C2[ppm]＝(A-B2)/A×106
The alkali-free glass of the present invention has a shrinkage rate C1 of 5ppm or less, and a shrinkage rate C2 of 40ppm or less
Since the shrinkage rates C1 and C2 of the alkali-free glass of the present invention satisfy the above-described conditions, it is possible to minimize deformation of the glass and dimensional changes associated with structural stabilization of the glass when exposed to high temperatures in the film forming process performed in the process of manufacturing various displays using the alkali-free glass.
In embodiment 1 of the alkali-free glass of the present invention, the shrinkage rate C1 is 5ppm or less, while the shrinkage rate C2 is 25ppm or less, more preferably 20ppm or less.
In the alkali-free glass of the invention according to mode 2, the shrinkage rate C1 is 5ppm or less, while the shrinkage rate C2 is 40ppm or less, more preferably 35ppm or less.
In addition, the alkali-free glass of the present invention preferably has a viscosity η of 10 in order to facilitate melting and to suppress erosion of refractory bricks constituting a melting furnace2Temperature T in poise (dPa · s)2Is 1760 ℃ or lower.
Here, in mode 1 of the alkali-free glass of the present invention, T2Preferably 1760 ℃ or lower, more preferably 1740 ℃ or lower, and still more preferably 1720 ℃ or lower.
In mode 2 of the alkali-free glass of the present invention, T2Preferably 1730 ℃ or lower, more preferably 1710 ℃ or lower, and still more preferably 1690 ℃ or lower.
In addition, the alkali-free glass of the present invention has a viscosity η of 10 for easy float forming4Temperature T in poise (dPa · s)4Preferably 1380 ℃ or lower.
Here, in mode 1 of the alkali-free glass of the present invention, T4Preferably 1380 ℃ or lower, more preferably 1360 DEG CHereinafter, more preferably 1340 ℃ or lower.
In mode 2 of the alkali-free glass of the present invention, T4Preferably 1360 ℃ or lower, more preferably 1340 ℃ or lower, and still more preferably 1320 ℃ or lower.
In addition, the alkali-free glass of the present invention preferably has an average thermal expansion coefficient of 40 × 10 at 50 to 350 ℃ for the purpose of improving thermal shock resistance and productivity in manufacturing a panel-7Below/° c.
In the alkali-free glass of the present invention, in mode 1, the average thermal expansion coefficient at 50 to 350 ℃ is preferably 37X 10-7/° C or less, more preferably 34X 10-7Below/° c.
In the alkali-free glass of the invention of claim 2, the average thermal expansion coefficient at 50 to 350 ℃ is preferably 40X 10-7Lower than/° C, more preferably 38X 10-7Below/° c.
The alkali-free glass of the present invention preferably has a glass transition temperature of 780 ℃ or higher in order to suppress thermal shrinkage during panel production and to enable application of a method based on laser annealing as a method for producing a p-Si TFT.
When the glass transition temperature is 780 ℃ or higher, it is suitable for applications in which the glass fictive temperature is likely to rise during the production process (for example, a display substrate or an illumination substrate for organic EL or the like having a plate thickness of 0.7mm or less, preferably 0.5mm or less, more preferably 0.3mm or less, or a display substrate or an illumination substrate for a thin plate having a plate thickness of 0.3mm or less, preferably 0.1mm or less).
In the molding of a sheet glass having a thickness of 0.7mm or less, further 0.5mm or less, further 0.3mm or less, further 0.1mm or less, the drawing speed during molding tends to be high, and therefore the virtual temperature of the glass tends to be high, and the shrinkage rate of the glass tends to be high. In this case, if the glass has a high glass transition temperature, the shrinkage can be suppressed.
The alkali-free glass of the present invention can be produced, for example, by the following method. The target components are prepared from the raw materials of the respective components which are generally used, and the target components are continuously charged into a furnace, heated to 1550 to 1650 ℃ and melted. The molten glass is formed into a predetermined thickness by a float process, annealed, and then cut to obtain a flat glass.
Examples
Examples 1 to 12 are examples, and examples 13 to 15 are comparative examples. The raw materials of each component are prepared into a target composition, and a platinum crucible is used for melting at the temperature of 1550-1650 ℃. During melting, the glass was homogenized by stirring with a platinum stirrer. Then, the molten glass is caused to flow out, formed into a plate shape, and annealed.
Tables 1 to 2 show the glass composition (% by mass) and the density ρ (g/cm)3) Young's modulus E (GPa) (measured by ultrasonic method), and specific elastic modulus E/rho (GP cm)3,/g), glass transition temperature Tg (unit: and an average thermal expansion coefficient alpha (unit: x 10-7/° c), the viscosity η of the glass reaches 102Temperature T in poise2(unit:. degree. C.) and a glass viscosity eta of 104Temperature T in poise4(unit:. degree. C.), and shrinkage ratios C1, C2 (unit: ppm, measured according to the above method).
In tables 1 to 2, the values shown in parentheses are calculated values.
Figure BDA0002004061460000111
Figure BDA0002004061460000121
As is clear from the table, the glass of examples had a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 40ppm or less. In addition, the average thermal expansion coefficient at 50-350 ℃ is 40 multiplied by 10-7Below/° c.
The present invention has been described in detail with reference to specific embodiments, but it is apparent to those skilled in the art that various changes or modifications can be made without departing from the spirit and scope of the invention.
The present application is based on japanese patent application 2013-134900, filed on 27.6.2013, the contents of which are incorporated herein by reference.
Industrial applicability
The alkali-free glass of the present invention is suitable as substrate glass for various displays or substrate glass for photomasks, and can also be used as a glass substrate for magnetic disks, etc. However, since the shrinkage ratio is low, it is effective as various display substrate glasses or photomask substrate glasses that are required to minimize deformation of glass and dimensional change accompanying structural stabilization of glass when exposed to high temperatures in a film forming process.

Claims (3)

1. An alkali-free glass having a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 40ppm or less,
the alkali-free glass contains, in mass% on an oxide basis:
Figure FDA0003254142680000011
MgO/(MgO + CaO) is not less than 0.20 and not more than 0.41, and
SiO2、Al2O3MgO and CaO in a total amount of 97 mass% or more, and
in the alkali-free glass, B2O3The content of (B) is 1 mass% or less,
the shrinkage ratio is a value measured by the following method:
first, a target glass is melted at 1550 to 1650 ℃, then the molten glass is caused to flow out, formed into a plate shape, cooled, and the obtained plate-shaped glass is polished to obtain a glass plate of 100mm × 20mm × 1mm,
next, the obtained glass plate was heated to a glass transition temperature Tg +70 ℃, held at this temperature for 1 minute, and then cooled to room temperature at a cooling rate of 40 ℃/minute, after which 2 indentations were made on the surface of the glass plate at intervals a in the longitudinal direction, the intervals a being 90mm, to thereby obtain a sample before treatment,
next, the sample before treatment was heated to 450 ℃ at a temperature rising rate of 100 ℃/hr, held at 450 ℃ for 2 hours, and then cooled to room temperature at a temperature falling rate of 100 ℃/hr to obtain a sample after treatment 1,
then, the indentation distance B1 of the treated sample 1 was measured,
from the A, B1 thus obtained, the shrinkage C1 was calculated using the formula:
C1＝(A-B1)/A×106c1 is in the ppm range;
further, the sample before treatment was heated to 600 ℃ at a temperature rising rate of 100 ℃/hr, held at 600 ℃ for 1 hour, and then cooled to room temperature at a temperature falling rate of 100 ℃/hr to obtain a sample after treatment 2,
then, indentation pitch B2 of sample 2 after treatment was measured,
from the A, B2 thus obtained, the shrinkage C2 was calculated using the formula:
C2＝(A-B2)/A×106and C2 is on the ppm scale.
2. The alkali-free glass according to claim 1, wherein the alkali-free glass has a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 25ppm or less,
the alkali-free glass contains, in mass% on an oxide basis:
Figure FDA0003254142680000021
and is
0.22≤MgO/(MgO+CaO)≤0.39。
3. The alkali-free glass according to claim 1, wherein the alkali-free glass has a shrinkage rate C1 of 5ppm or less and a shrinkage rate C2 of 40ppm or less,
the alkali-free glass contains, in mass% on an oxide basis:
Figure FDA0003254142680000022
and is
0.22≤MgO/(MgO+CaO)≤0.39。
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KR20160023700A (en) 2016-03-03
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KR102229428B1 (en) 2021-03-18
CN105324342A (en) 2016-02-10

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