WO2021117360A1 - Procédé de fabrication de verre d'aluminoborosilicate alcalino-terreux - Google Patents

Procédé de fabrication de verre d'aluminoborosilicate alcalino-terreux Download PDF

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Publication number
WO2021117360A1
WO2021117360A1 PCT/JP2020/040047 JP2020040047W WO2021117360A1 WO 2021117360 A1 WO2021117360 A1 WO 2021117360A1 JP 2020040047 W JP2020040047 W JP 2020040047W WO 2021117360 A1 WO2021117360 A1 WO 2021117360A1
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WIPO (PCT)
Prior art keywords
glass
alkaline earth
raw material
content
aluminum borosilicate
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PCT/JP2020/040047
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English (en)
Japanese (ja)
Inventor
真人 六車
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日本電気硝子株式会社
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Publication of WO2021117360A1 publication Critical patent/WO2021117360A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B1/00—Preparing the batches
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B17/00—Forming molten glass by flowing-out, pushing-out, extruding or drawing downwardly or laterally from forming slits or by overflowing over lips
    • C03B17/06—Forming glass sheets
    • 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
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333—Constructional arrangements; Manufacturing methods
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/02—Details
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
    • H10K77/10—Substrates, e.g. flexible substrates

Definitions

  • the present invention relates to a method for producing alkaline earth aluminum borosilicate glass, and more particularly to a method for producing alkaline earth aluminum borosilicate glass used for a substrate of a liquid crystal display or an organic EL display.
  • a non-alkali glass plate that is, a non-alkali alkaline earth aluminum borosilicate glass plate has been used for a substrate such as a liquid crystal display.
  • liquid crystal displays or organic EL display substrates have been required to have the property of being resistant to heat shrinkage due to heat treatment in the display manufacturing process. In order to reduce the amount of heat shrinkage, it is effective to increase the strain point of the glass plate.
  • Patent Document 1 discloses that by reducing the content of B 2 O 3 in the glass composition, the strain point of the glass plate is increased and heat shrinkage is made difficult.
  • non-alkali glass with a high strain point is easy to melt and separate when the glass raw material is melted, so stable production is difficult.
  • the present invention has been made in view of the above circumstances, and the technical problem thereof is that the alkaline earth aluminum borosilicate which is hard to be melt-separated when the glass raw material is melted and which is hard to be heat-shrinked by the heat treatment in the display manufacturing process. It is to devise a method for producing acid glass.
  • the present inventor has found that the above technical problems can be solved by using borax as a boron-introducing raw material for alkaline earth aluminoborosilicate glass, and proposes it as the present invention. That is, the method for producing alkaline earth aluminum borosilicate glass of the present invention is a boron-introduced raw material so that alkaline earth aluminum borosilicate glass having an alkali metal oxide content of 0.01 to 1% by mass can be obtained.
  • boric acid H 3 BO 3
  • anhydrous boric acid B 2 O 3
  • boric acid H 3 BO 3
  • B 2 O 3 anhydrous boric acid
  • the amount of water in the glass is reduced to increase the strain point of the glass plate
  • anhydrous boric acid is used, but in that case, the batch cost increases.
  • anhydrous borax Na 2 O ⁇ 2B 2 O 3
  • the amount of water in the glass can be reduced at low cost, but Na 2 O is introduced into the glass at the same time.
  • Anhydrous borax Na 2 O ⁇ 2B 2 O 3
  • alkaline earth elements Mg, Ca, Sr, Ba
  • Alkaline earth oxide melt has high density and low viscosity, so melt separation occurs.
  • boric acid raw material boric acid raw material
  • borax raw material borax raw material
  • the borax raw material contains an alkaline component (Na 2 O) that deteriorates the characteristics of the display.
  • Na 2 O alkaline component
  • the content of B 2 O 3 in the alkaline earth aluminum borosilicate glass is preferably 0.1 to 5% by mass.
  • the SO 3 content in the alkaline earth aluminum borosilicate glass is preferably 0.01% by mass or less.
  • the method for producing alkaline earth aluminum borosilicate glass of the present invention it is preferable to mold the molten glass into a plate shape by an overflow down draw method.
  • molten glass is formed into a plate shape to obtain a glass plate of alkaline earth aluminum borosilicate glass, and then the glass plate is displayed on a liquid crystal display or organic. It is preferably used as a substrate for an EL display.
  • the data shows that the initial melt of sodium borate has a lower viscosity than the initial melt of borate in the temperature range of about 800 ° C. where the initial melt is formed, and the source of the data is J. . Am. Ceram. Soc. Vol.36 (1953) p.319.
  • Sample No. in the column of Examples. It is XRF data which showed the content ( ⁇ RO) of alkaline earth metal oxide of each cross section of glass about 1 and 2.
  • Sample No. in the column of Examples. It is the XRF data which showed the content ( ⁇ RO) of the alkaline earth metal oxide of each cross section of the glass about 3-5.
  • Sample No. in the column of Examples. About 3-5 is data XRF indicated the content of SO 3 of each cross section of the glass.
  • Sample No. in the column of Examples. It is the data which showed the ratio of the total amount of MgO and CaO of each cross section of the glass about 3-5.
  • Sample No. in the column of Examples. It is the data which showed the ratio of the total amount of SrO and BaO of each cross section of the glass about 3-5.
  • the method for producing an alkaline earth aluminum borosilicate glass of the present invention contains a boron-introduced raw material so that an alkaline earth aluminum borosilicate glass having an alkali metal oxide content of 0.01 to 1% by mass can be obtained.
  • the method for producing the alkaline earth aluminum borosilicate glass of the present invention will be described in detail.
  • a borax material to all or part of the boron introduced raw material, preferably a majority of the content of B 2 O 3 in the glass composition is introduced by borax material More preferably, 80% or more of the content of B 2 O 3 in the glass composition is introduced as a borax raw material.
  • the borax raw material is used, an initial melt of sodium borate is formed when the glass raw material is melted. Since the initial melt of sodium borate has a high contact frequency with the alkaline earth element, it is easy to take in the alkaline earth element, and the formation of the melt of the alkaline earth oxide is suppressed. As a result, melt separation can be effectively suppressed.
  • the raw materials for introducing alkaline earth oxides are oxides of alkaline earth elements, carbonates, nitrates, hydroxides, sulfates, halides or double salts thereof.
  • the raw material for introducing the alkaline earth oxide is an easily meltable component in a glass batch of alkaline earth aluminosilicate glass, and the alkaline earth oxide melt has a density higher than that of the molten glass and a low viscosity. Therefore, the alkaline earth oxide melt is likely to sink when the glass raw material is dissolved, and the SrO melt and the BaO melt are particularly likely to sink.
  • the glass composition is SiO 2 50 to 70%, Al 2 O 3 10 to 25%, B 2 O 30 in terms of the following oxide-equivalent mass%.
  • the glass raw materials are mixed and mixed so as to contain 1 to 15%, Li 2 O + Na 2 O + K 2 O 0.01 to 1%, MgO 0 to 8%, CaO 3 to 10%, and SrO + BaO 0.1 to 20%. Then, it is preferable to prepare a glass batch.
  • the reasons for limiting the glass composition as described above are shown below. In the description of the content range of each component, the% indication indicates mass%.
  • SiO 2 is a component that forms the skeleton of glass.
  • the content of SiO 2 is preferably 50 to 70%, 54 to 68%, 56 to 66%, and particularly 58 to 64%. If the content of SiO 2 is too small, the density becomes too high and the acid resistance tends to decrease. On the other hand, if the content of SiO 2 is too large, the high-temperature viscosity tends to increase and the meltability tends to decrease, and devitrified crystals such as cristobalite tend to precipitate, so that the liquidus temperature tends to rise. Become.
  • B 2 O 3 is a component that enhances meltability and devitrification resistance.
  • the content of B 2 O 3 is preferably 0 to 15%, 0.1 to 6%, 0.3 to 3%, and particularly 0.5 to 2.3%. If the content of B 2 O 3 is too small, the meltability and devitrification resistance tend to decrease, and the resistance to hydrofluoric acid-based chemicals tends to decrease. On the other hand, if the content of B 2 O 3 is too large, Young's modulus and strain point tend to decrease.
  • Alkali metal oxides (Li 2 O, Na 2 O, K 2 O) are essential components for using borax raw materials, and are components that lower the melting temperature and molding temperature. However, if the content of the alkali metal oxide is too high, the performance of the display will be adversely affected. Therefore, the content of Li 2 O + Na 2 O + K 2 O (the total amount of Li 2 O, Na 2 O and K 2 O) is preferably 0.01 to 1%, 0.02 to 0.2%, 0. It is 03 to 0.1%, especially 0.04 to 0.09%. In particular, the content of Na 2 O is preferably 0.01 to 1%, 0.02 to 0.2%, 0.03 to 0.1%, and particularly 0.04 to 0.09%.
  • the alkali metal oxide is mainly introduced from the borax raw material, but the alkali metal oxide may be introduced from a glass raw material other than the borax raw material.
  • an alkali metal oxide may be introduced from a glass raw material such as a lithium salt, a sodium salt, or a potassium salt.
  • MgO is a component that lowers high-temperature viscosity and enhances meltability, and is a component that significantly increases Young's modulus among alkaline earth metal oxides.
  • the content of MgO is preferably 0 to 8%, 0 to 7%, 0 to 6%, 0 to 3%, and particularly 0 to 2%. If the content of MgO is too small, the meltability and Young's modulus tend to decrease. On the other hand, if the content of MgO is too large, the devitrification resistance tends to decrease and the strain point tends to decrease.
  • CaO is a component that lowers high-temperature viscosity and remarkably enhances meltability without lowering the strain point. Further, among alkaline earth metal oxides, since the introduced raw material is relatively inexpensive, it is a component that reduces the raw material cost.
  • the CaO content is preferably 3 to 10%, 4 to 10%, and particularly 5 to 9%. If the CaO content is too low, it becomes difficult to enjoy the above effects. On the other hand, if the CaO content is too high, the glass tends to be devitrified and the coefficient of thermal expansion tends to be high.
  • SrO and BaO are components that enhance devitrification resistance, but are components that promote melt separation. Further, it is a component that lowers the high-temperature viscosity without lowering the strain point, enhances the meltability, and suppresses the rise in the liquidus temperature.
  • the content of SrO + BaO (the total amount of SrO and BaO) is preferably 0.1 to 25%, 1 to 22%, 2 to 20%, and particularly 5 to 18%. In particular, the content of SrO is preferably 0 to 8%, 0.1 to 7%, and particularly 0.5 to 6%.
  • the content of BaO is preferably 0 to 20%, 0.1 to 18%, 1 to 17%, 3 to 16%, and particularly 5 to 15%.
  • SnO 2 is a component that acts as a fining agent, and its content is preferably 0 to 1%, 0.1 to 0.5%, and particularly 0.2 to 0.4%. If the content of SnO 2 is too large, devitrified crystals are likely to precipitate, and the liquidus temperature is likely to rise.
  • SO 3 is a component that causes foam defects due to riboyl of SO 2 gas.
  • the content of SO 3 is preferably 0.01% or less, preferably 0.005% or less. If the content of SO 3 is too large, foam defects due to riboyl of SO 2 gas are likely to occur.
  • the content of the components other than the above components is preferably 10% or less, particularly 5% or less in total, from the viewpoint of accurately enjoying the effects of the present invention.
  • the strain point is preferably 700 ° C. or higher, 720 ° C. or higher, and particularly preferably 740 to 850 ° C. If the strain point is too low, the glass plate tends to shrink due to heat treatment in the display manufacturing process. On the other hand, if the strain point is too high, the manufacturing cost of the glass plate tends to rise.
  • the temperature at 10 2.5 dPa ⁇ s is preferably 1530 to 1680 ° C, more preferably 1550 to 1650 ° C, and particularly preferably 1580 to 1630 ° C. If the temperature at 10 2.5 dPa ⁇ s is too low, the glass plate tends to shrink due to heat treatment in the display manufacturing process. On the other hand, if the temperature at 10 2.5 dPa ⁇ s is too high, the meltability is lowered and the manufacturing cost of the glass plate is likely to rise.
  • the "temperatur at 10 2.5 dPa ⁇ s" can be measured by a well-known platinum ball pulling method.
  • the obtained glass batch is put into a melting furnace.
  • the glass batch is usually continuously charged into the melting furnace by a raw material feeder such as a screw charger, but may be intermittently charged.
  • the glass batch put into the melting furnace is heated by the combustion atmosphere of a burner or the like or the electrodes installed inside the melting furnace to become molten glass.
  • the melting temperature of the glass raw material is about 1530 to 1680 ° C.
  • the obtained molten glass is subjected to a clarification step, a stirring step, and a supply step, and then gradually cooled for charging into a molding apparatus.
  • the molten glass is supplied to a molding apparatus, formed into a plate shape having a predetermined wall thickness and surface quality, and then cut into a predetermined size to become a glass product (glass plate).
  • a molding method an overflow down draw method, a float method, or the like can be adopted.
  • the overflow down draw method is preferable because it can produce an unpolished and smooth-surfaced glass plate.
  • the glass plate thus produced is suitably used as a substrate for, for example, a liquid crystal display, an organic EL display, or the like.
  • Each sample was prepared as follows. Glass raw materials were mixed so as to have the glass composition shown in the table, and a glass batch corresponding to 100 g of glass was prepared. The glass raw materials in the table were used as the raw materials for introducing Na 2 O and B 2 O 3. Other glass raw materials are sample No. The same thing was used in 1-5.
  • the obtained glass batch was put into a triangular crucible (conical platinum alloy crucible), melted at 1600 ° C. for 2 hours, and then rapidly cooled. Then, the glass was peeled off from the triangular crucible, and the glass composition of the cross section of the glass 5 mm, 15 mm, and 21 mm from the top was analyzed by XRF. The results are shown in FIGS. 2-9.
  • FIG. 2-9 The results are shown in FIGS. 2-9.
  • FIG. 2 shows the sample No. It is XRF data which showed the content ( ⁇ RO) of alkaline earth metal oxide of each cross section of glass about 1 and 2.
  • FIG. 3 shows the sample No. For 1,2, a data of XRF indicated the content of SO 3 of each cross section of the glass.
  • FIG. 4 shows the sample No. It is the XRF data which showed the content ( ⁇ RO) of the alkaline earth metal oxide of each cross section of the glass about 3-5.
  • FIG. 5 shows the sample No. About 3-5 is data XRF indicated the content of SO 3 of each cross section of the glass.
  • FIG. 6 shows the sample No. For 1 and 2, it is the data which showed the ratio of the total amount of MgO and CaO of each cross section of glass.
  • FIG. 7 shows the sample No.
  • FIG. 8 shows the sample No. It is the data which showed the ratio of the total amount of MgO and CaO of each cross section of glass about 3-5.
  • FIG. 9 shows the sample No. It is the data which showed the ratio of the total amount of SrO and BaO of each cross section of the glass about 3-5.
  • the vertical axis of FIGS. 6 and 8 shows the ratio of the total amount of MgO and CaO when the total amount of MgO and CaO in the cross section of the glass 5 mm from the top is 1.
  • the vertical axis of FIGS. 7 and 9 shows the ratio of the total amount of SrO and BaO when the total amount of SrO and BaO in the cross section of the glass 5 mm from the top is 1.
  • alkaline earth aluminoborosilicate glass having a B 2 O 3 content of 0.8% by mass tends to undergo melt separation, but when a borax raw material is used, the degree of melt separation occurs. Is improved, and the uneven distribution of SO 3 is also improved.
  • the alkaline earth aluminoborosilicate glass which is the content of B 2 O 3 is 6.5 wt%, hardly occurs melt separation hardly unevenly distributed SO 3, borax The need to use raw materials is not high.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nonlinear Science (AREA)
  • Mathematical Physics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Glass Compositions (AREA)
  • Liquid Crystal (AREA)
  • Electroluminescent Light Sources (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

La présente invention concerne un procédé de fabrication de verre d'aluminoborosilicate alcalino-terreux qui est caractérisé en ce qu'il comprend les étapes suivantes : le mélange, une composition étant préparée par mélange de matières premières de verre, qui comprennent une matière première d'introduction de bore, de façon à obtenir du verre d'aluminoborosilicate alcalino-terreux dont la teneur en oxyde de métal alcalin est comprise entre 0,01 % en masse et 1 % en masse ; la fusion, la composition étant introduite dans un four de fusion, ce qui permet d'obtenir du verre fondu ; le moulage, le verre fondu étant moulé en une plaque, ce qui permet d'obtenir du verre d'aluminoborosilicate alcalino-terreux. Ce procédé de fabrication de verre d'aluminoborosilicate alcalino-terreux est également caractérisé en ce qu'une matière première à base de borax est utilisée en tant que partie ou totalité de la matière première d'introduction de bore.
PCT/JP2020/040047 2019-12-10 2020-10-26 Procédé de fabrication de verre d'aluminoborosilicate alcalino-terreux WO2021117360A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114685044A (zh) * 2022-03-18 2022-07-01 安徽汉柔光电科技有限公司 一种易熔高化学稳定性的碱铝硅玻璃

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5398318A (en) * 1977-02-02 1978-08-28 Owens Corning Fiberglass Corp Production of glass
JPH0333025A (ja) * 1989-06-29 1991-02-13 Nippon Electric Glass Co Ltd 低アルカリガラス用原料組成物
JP2005537211A (ja) * 2002-08-29 2005-12-08 コーニング インコーポレイテッド ガス発生フリットを用いたガラスの製造
JP2009280425A (ja) * 2008-05-21 2009-12-03 Sharp Corp 無アルカリガラスのリサイクル方法およびそれにより得られるガラス材料
JP2009295593A (ja) * 2003-08-08 2009-12-17 Nippon Electric Glass Co Ltd 外部電極蛍光ランプ用外套容器
JP2014519464A (ja) * 2011-04-29 2014-08-14 ユーロケラ ソシエテ オン ノーム コレクティフ 電磁調理器具
JP2019119615A (ja) * 2017-12-28 2019-07-22 日本電気硝子株式会社 ガラスの製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5398318A (en) * 1977-02-02 1978-08-28 Owens Corning Fiberglass Corp Production of glass
JPH0333025A (ja) * 1989-06-29 1991-02-13 Nippon Electric Glass Co Ltd 低アルカリガラス用原料組成物
JP2005537211A (ja) * 2002-08-29 2005-12-08 コーニング インコーポレイテッド ガス発生フリットを用いたガラスの製造
JP2009295593A (ja) * 2003-08-08 2009-12-17 Nippon Electric Glass Co Ltd 外部電極蛍光ランプ用外套容器
JP2009280425A (ja) * 2008-05-21 2009-12-03 Sharp Corp 無アルカリガラスのリサイクル方法およびそれにより得られるガラス材料
JP2014519464A (ja) * 2011-04-29 2014-08-14 ユーロケラ ソシエテ オン ノーム コレクティフ 電磁調理器具
JP2019119615A (ja) * 2017-12-28 2019-07-22 日本電気硝子株式会社 ガラスの製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114685044A (zh) * 2022-03-18 2022-07-01 安徽汉柔光电科技有限公司 一种易熔高化学稳定性的碱铝硅玻璃

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