WO2012132449A1 - ガラス基板の製造方法 - Google Patents
ガラス基板の製造方法 Download PDFInfo
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- WO2012132449A1 WO2012132449A1 PCT/JP2012/002180 JP2012002180W WO2012132449A1 WO 2012132449 A1 WO2012132449 A1 WO 2012132449A1 JP 2012002180 W JP2012002180 W JP 2012002180W WO 2012132449 A1 WO2012132449 A1 WO 2012132449A1
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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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
- C03C3/089—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 relates to a method for producing a glass substrate containing SiO 2 and Fe 2 O 3 and having a SiO 2 content of 50 to 70% by mass.
- a liquid crystal panel used in a liquid crystal display device is mainly composed of two substrates and a liquid crystal material between them. More specifically, in a liquid crystal panel, a liquid crystal material is provided between a substrate in which a color filter is formed on a glass substrate and a substrate in which a semiconductor element such as a TFT (Thin Film Transistor) is formed on the glass substrate. It is manufactured by being sandwiched and sealed around the substrate with a sealant. In the process of manufacturing a liquid crystal panel, irradiation with ultraviolet rays (wavelength 300 to 380 nm) is performed through a glass substrate.
- TFT Thin Film Transistor
- ultraviolet rays (wavelength 300 to 380 nm) are irradiated through a glass substrate, and the periphery of the substrate is sealed with lithography or ultraviolet curable resin.
- a method of stabilizing the alignment of liquid crystal molecules by irradiating ultraviolet rays through a glass substrate to polymerize a photopolymerized polymer in the liquid crystal material is also used.
- ultraviolet rays having a wavelength of about 300 nm are often used, and in particular, it is desired to improve the ultraviolet transmittance near the wavelength of 300 nm.
- arsenic oxide (As 2 O 3 ) and antimony oxide (Sb 2 O 3 ) are not used from the viewpoint of environmental load in the glass substrate used for the liquid crystal display element, and tin oxide (SnO 2 ) or iron oxide (Fe It is known to use 2 O 3 ) as a fining agent (Patent Document 1). It is also known that in this glass substrate, the occurrence frequency of defect levels due to bubbles in the glass substrate can be dramatically reduced by increasing the content of Fe 2 O 3 from a predetermined value.
- the present invention provides a glass substrate capable of efficiently producing a glass substrate having a transmittance of 30% or more at a wavelength of 300 nm while sufficiently clarifying the glass when producing a glass substrate for a liquid crystal display device.
- An object is to provide a manufacturing method.
- SiO 2 content is method of manufacturing a glass substrate for a liquid crystal display device is 50 to 70 mass%.
- the illegal manufacturing is A raw material preparation step for preparing a glass raw material by using at least a silica raw material mainly composed of SiO 2 and a preparation raw material containing iron oxide, A melting step of melting the glass raw material into a molten glass; And a refining step for refining the molten glass.
- the silica raw material contains iron oxide as an impurity, and when the iron oxide is represented by Fe 2 O 3 , the silica raw material contains 0.001 to 0.028 mass% of Fe 2 O 3 , Content in the said glass raw material is adjusted so that the transmittance
- the said content of the said adjustment raw material is further adjusted according to the clarification effect in the said clarification process of the said molten glass.
- the content of Fe 2 O 3 contained in the glass substrate derived from the impurities of the silica raw material is 50% by mass or less with respect to the content of Fe 2 O 3 contained in the glass substrate to be produced. Is preferable.
- the glass substrate contains 1 to 10% by mass of CaO
- the glass raw material includes limestone that is a raw material for the CaO
- the limestone contains iron oxide as an impurity, and when the iron oxide contained in the limestone is represented by Fe 2 O 3 , the limestone contains 0.001 to 0.05 mass% of Fe 2 O 3
- the silica raw material used for the glass raw material preferably contains 0.001 to 0.015 mass% of Fe 2 O 3 .
- the glass substrate contains 1 to 15% by mass of CaO
- the glass raw material includes limestone that is a raw material for the CaO
- the limestone contains iron oxide as an impurity, and when the iron oxide contained in the limestone is represented by Fe 2 O 3 , the limestone contains 0.001 to 0.05 mass% of Fe 2 O 3
- the silica raw material used for the glass raw material preferably contains 0.001 to 0.0125% by mass of Fe 2 O 3 .
- the content of Fe 2 O 3 contained in the glass substrate derived from the impurities of the silica raw material and the limestone is 50% by mass or less with respect to the content of Fe 2 O 3 contained in the glass substrate to be produced.
- the glass substrate preferably contains 0.15 to 0.25% by mass of SnO 2 .
- the ⁇ -OH value contained in the glass substrate to be produced is 0.45 / mm or less. It is preferable that the glass substrate is substantially free of As 2 O 3 and Sb 2 O 3 .
- Another embodiment of the present invention is a method for producing a glass substrate for a liquid crystal display device containing SiO 2 and Fe 2 O 3 and having a SiO 2 content of 50 to 70 mass%.
- the manufacturing method is A raw material preparation step of preparing a glass raw material containing at least a silica raw material mainly composed of SiO 2 ; Melting the glass raw material to form a molten glass; And a refining step for refining the molten glass.
- the silica raw material contains iron oxide as an impurity, and when the iron oxide is represented by Fe 2 O 3 , the silica raw material contains 0.001 to 0.028 mass% of Fe 2 O 3 .
- the glass raw material is prepared using an adjustment raw material containing iron oxide in the raw material preparation step.
- Another embodiment of the present invention is a liquid crystal display device containing SiO 2 and Fe 2 O 3 , having a SiO 2 content of 50 to 70% by mass, and a transmittance at a wavelength of 300 nm of 30% or more. It is a manufacturing method of the glass substrate for water.
- the manufacturing method is A raw material preparation step of preparing a glass raw material by using at least a silica raw material containing SiO 2 as a main component and iron oxide as an impurity, and a preparation raw material containing iron oxide as a main component, Melting the glass raw material to form a molten glass; And a refining step for refining the molten glass.
- the iron oxide contained as an impurity in the silica raw material is represented by Fe 2 O 3
- the silica raw material contains 0.001 to 0.028 mass% of the Fe 2 O 3 .
- the glass substrate can be sufficiently clarified and a glass substrate having a transmittance of 30% or more at a wavelength of 300 nm can be stably produced.
- the glass substrate manufactured by the manufacturing method of the glass substrate for liquid crystal display devices of the present embodiment (hereinafter simply referred to as a glass substrate) will be described.
- the glass substrate is a glass substrate for a liquid crystal display device containing 50 to 70% by mass of SiO 2 and is used for two glass substrates sandwiching a liquid crystal material of a liquid crystal panel.
- the thickness of the glass substrate is, for example, 0.3 to 0.7 mm, and the size is 300 ⁇ 400 mm to 2200 ⁇ 2500 mm.
- the transmittance of the glass substrate is 30% or more at a wavelength of 300 nm.
- the transmittance at a wavelength of 300 nm is 30% or more.
- the transmittance at a wavelength of 300 nm is 30% or more regardless of the thickness. It means that.
- the transmittance of the glass substrate is set to the above value when the liquid crystal panel is manufactured by irradiating ultraviolet rays having a wavelength of 300 nm, for example, by polymerizing a photopolymerized polymer in a liquid crystal material and aligning liquid crystal molecules. This is to efficiently perform the process of stabilizing.
- the ⁇ -OH value of the glass substrate is preferably 0.45 / mm or less. When the ⁇ -OH value exceeds 0.45 / mm, the occurrence frequency of defects due to bubbles generated in the glass substrate increases.
- the glass substrate examples include aluminoborosilicate glass having the composition shown below.
- the numerical value described in the following parenthesis is a preferable composition ratio.
- % means mass%.
- SiO 2 50 to 70% (55 to 68%, 58 to 62%), Al 2 O 3 : 10 to 25% (15 to 20%, 15 to 18%), B 2 O 3 : 4 to 18% (6 to 14%, 10 to 13%), MgO: 0-10% (0-5%, 1-2%)
- K 2 O 0 to 2% (0.1 to 2%, 0.1 to 0.5%)
- SnO 2 0 to 1% (0.01 to 0.5%, 0.05 to 0.4%, 0.1 to 0.3%, 0.15 to 0.25%
- Fe 2 O 3 0.01 to 0.045% (0.015 to 0.04%, 0.02 to
- an aluminoborosilicate glass having the composition shown below can be mentioned.
- SiO 2 50 to 70% (55 to 68%, 58 to 63%), Al 2 O 3 : 8 to 25% (10 to 23%, 14 to 23%), B 2 O 3 : 3 to 15% (5 to 15%, 6 to 13%), MgO: 0 to 10% (0 to 7%, 0 to 1%), CaO: 0 to 20% (4 to 14%, 5 to 12%), SrO: 0 to 20% (0 to 10%, 0 to 1%), BaO: 0 to 10% (0 to 2%, 0 to 1%), K 2 O: 0 to 2% (0.1 to 2%, 0.1 to 0.5%), SnO 2 : 0 to 1% (0.01 to 0.5%, 0.05 to 0.4%, 0.1 to 0.3%, 0.15 to 0.25%), Fe 2 O 3 : 0.01 to 0.045% (0.015 to 0.04%, 0.02 to 0.035%).
- SnO 2 is preferably 0.15 to 0.25% from the viewpoint of improving the transmittance of ultraviolet rays.
- silica sand containing 0.028% by mass or less of Fe 2 O 3 as an impurity is used as the silica raw material that is SiO 2 .
- the content of Fe 2 O 3 is (in terms of the) value expressed in Fe 2 O 3 in total oxides such as Fe 2+ and Fe 3+.
- the transmittance referred to in the present invention is a value obtained by measuring the transmittance at a wavelength of 200 nm to 800 nm on this glass specimen using a spectrophotometer.
- a spectrophotometer For example, “UV-3100PC” manufactured by Shimadzu Corporation is used as the spectrophotometer.
- the ⁇ -OH value is a measure of the hydroxyl group content in the glass measured by IR spectroscopy, and is a measure of the moisture in the glass.
- the ⁇ -OH value is determined according to the following formula.
- ⁇ -OH value (1 / W) LOG 10 (T 1 / T 2 )
- W is the thickness (mm) of the sample.
- SiO 2 is a component constituting the glass skeleton of the glass substrate, and has the effect of increasing the chemical durability and heat resistance of the glass.
- the SiO 2 content is too low, the effects of chemical durability and heat resistance are not sufficiently obtained, and when the SiO 2 content is too high, the glass tends to be devitrified, making molding difficult, The viscosity increases and it becomes difficult to clarify and homogenize the glass.
- Al 2 O 3 is a component that forms a glass skeleton, and has an effect of increasing the chemical durability and heat resistance of the glass. If the Al 2 O 3 content is too low, the effects of chemical durability and heat resistance of the glass cannot be obtained sufficiently. On the other hand, if the Al 2 O 3 content is too high, the viscosity of the glass is increased and melting becomes difficult, and the acid resistance decreases.
- B 2 O 3 is a component that lowers the viscosity of the glass and promotes melting and clarification of the glass. If the content of B 2 O 3 is too low, the viscosity of the glass becomes high and it becomes difficult to homogenize the glass. If the content of B 2 O 3 is too high, the heat resistance of the glass, the chemical resistance decreases.
- MgO and CaO are components that lower the viscosity of the glass and promote glass melting and fining. Further, MgO and CaO are advantageous components for improving the meltability while reducing the weight of the obtained glass because the ratio of increasing the density of the glass is small in the alkaline earth metal oxide. However, if the MgO and CaO content is too high, devitrification is likely to occur and the chemical durability of the glass is lowered.
- SrO and BaO are components that lower the viscosity of the glass and promote the melting and clarification of the glass. Moreover, it is also a component which improves the oxidizability of a glass raw material and improves clarity. However, if the content of SrO and BaO is too high, the density of the glass increases, the weight of the glass plate cannot be reduced, and the chemical durability of the glass decreases.
- K 2 O is a component that lowers the high-temperature viscosity of the glass and improves the meltability and moldability of the glass and at the same time improves the devitrification resistance. However, if the content of K 2 O becomes too high, the coefficient of thermal expansion becomes too high.
- SnO 2 is used as a glass refining agent because it causes a reaction with valence fluctuation in molten glass.
- SnO 2 is a component that makes glass easily devitrified, its content is preferably 0.01 to 0.5% by mass in order to prevent devitrification while enhancing clarity. It is more preferably 0.05 to 0.4% by mass, and further preferably 0.1 to 0.3% by mass.
- SnO 2 is preferably 0.15 to 0.25% by mass.
- Fe 2 O 3 is used as a glass refining agent because it causes a reaction with valence fluctuation in molten glass.
- a predetermined value specifically 0.02 mass% to 0.03 mass% (200 ppm to 300 ppm)
- a clarification effect is rapidly exerted. Reduce air bubbles.
- the ultraviolet transmittance decreases. Therefore, the glass substrate to be produced, the content of Fe 2 O 3 (wt%) is limited to a predetermined range.
- As 2 O 3 and Sb 2 O 3 are substances having an effect of causing a reaction with valence fluctuation in the molten glass and clarifying the glass, but As 2 O 3 and Sb 2 O 3 are environmental loads. Therefore, in the glass substrate of this embodiment, As 2 O 3 and Sb 2 O 3 are not substantially contained in the glass.
- the phrase “substantially free of As 2 O 3 and Sb 2 O 3” means that it is less than 0.1% by mass and is not intentionally contained.
- Such a glass substrate includes silica raw material containing SiO 2 as a main component (component of 98% by mass or more), alumina, CaCO 3 containing Al 2 O 3 as a main component (component of 98% by mass or more), and CaCO 3 .
- silica raw material containing SiO 2 as a main component (component of 98% by mass or more)
- alumina containing CaCO 3 containing Al 2 O 3 as a main component (component of 98% by mass or more)
- CaCO 3 a glass substrate
- silica raw material containing SiO 2 as a main component (component of 98% by mass or more)
- alumina e.g., CaCO 3 containing Al 2 O 3
- CaCO 3 e.g., CaCO 3 e.
- a small amount of iron oxide is contained as an impurity in silica raw material, alumina mainly composed of Al 2 O 3 , limestone mainly composed of CaCO 3 and the like.
- an impurity is not the component contained intentionally but the component which is not intended with respect to a raw material and contains 0.5 mass% or less.
- these raw materials by suppressing the content of iron oxide in the silica raw material that is the raw material of SiO 2 having the highest content in the glass substrate, the properties of the glass substrate (chemical durability, heat resistance, While maintaining acid resistance, devitrification resistance, viscosity of the molten glass, etc.), the clarification effect in the clarification step described later can be easily controlled, and a glass substrate having a transmittance of 30% or more at a wavelength of 300 nm is efficient. Can be manufactured well.
- the content of Fe 2 O 3 in the silica raw material is represented by Fe 2 O 3 (hereinafter simply referred to as the content of Fe 2 O 3 in the silica raw material)
- the content of Fe 2 O 3 kept pre-way below figures the content of Fe 2 O 3 where fining effect of the molten glass is rapidly improved, the determination of the frequency of occurrence of defects due to bubbles in the glass substrate produced at this time
- the glass raw material is blended and adjusted using the raw material containing iron oxide as the adjusting raw material so as to increase the content of Fe 2 O 3 in the molten glass.
- the blending amount of the adjustment raw material for blending adjustment is limited so that the transmittance in the vicinity of the wavelength of 300 nm is 30% or more.
- the adjustment raw material for adjusting the blend include ferric oxide (Bengara) containing Fe 2 O 3 as a main component (a component containing 95% by mass or more).
- a raw material containing iron oxide such as alumina or limestone as an impurity can be included in the glass raw material before blending adjustment.
- the content of iron oxide in the molten glass is suppressed to a value lower than the value of the content of Fe 2 O 3 that sharply improves the clarification effect of the molten glass.
- the raw material containing iron oxide (adjusted raw material) is added to the glass raw material containing raw materials such as silica or limestone according to the clarification effect of the molten glass at the time of glass substrate production, and blending adjustment To do.
- the silica raw material mainly composed of SiO 2 and the adjustment raw material containing iron oxide are mixed with other raw materials. Mix with raw materials to make glass raw materials. This glass raw material is melted to obtain molten glass. Thereafter, the molten glass is clarified. At this time, the silica raw material contains iron oxide. When this iron oxide is represented by Fe 2 O 3 , the silica raw material contains 0.028% by mass or less of Fe 2 O 3 as impurities. The content of the adjustment raw material contained in the glass raw material in the glass raw material is adjusted so that the transmittance of ultraviolet rays is 30% or more.
- the content of such adjustment material as described below, the content of Fe 2 O 3 in the molten glass, a little over a number of the content of Fe 2 O 3 where fining effect is abruptly improved As adjusted. Thereby, the transmittance at a wavelength of 300 nm can be adjusted to be 30% or more. Therefore, Fe content of 2 O 3 is incorporated adjustment of the adjustment feedstock fining effect by Fe 2 O 3 in the molten glass is required to exceed slightly the values for the content of Fe 2 O 3 at the time of rapidly improved It is necessary to find the amount. On the other hand, the content value of Fe 2 O 3 when the clarification effect by Fe 2 O 3 in the molten glass is rapidly improved varies depending on the composition of the glass substrate.
- the silica raw material 0.028% by weight of Fe 2 O 3 as an impurity (the iron oxide Fe 2 O 3
- the content ratio is as follows: Thereby, the content rate of Fe 2 O 3 derived from the silica raw material contained in the molten glass is the content of the Fe 2 O 3 content when the clarification effect by Fe 2 O 3 in the molten glass is rapidly improved. Can be lower than the value.
- FIG. 1 is a diagram illustrating an example of a flow of a method for manufacturing a glass substrate according to the present embodiment.
- the glass plate manufacturing method includes a raw material preparation step (step S5), a melting step (step S10), a clarification step (step S20), a stirring step (step S30), a forming step (step S40), and a slow cooling. It mainly includes a process (step S50), a plate-drawing process (step S60), a shape processing process (step S70), and an inspection process (step S80).
- a silica raw material containing SiO 2 as a main component and an adjustment raw material containing iron oxide are prepared together with other raw materials to produce a glass raw material.
- the silica raw material used as the glass raw material contains iron oxide as an impurity, and the content of Fe 2 O 3 in the silica raw material is 0.028% by mass or less.
- the content of Fe 2 O 3 is preferably 0.02% by mass or less, and more preferably 0.015% by mass or less.
- it is preferable that the content of Fe 2 O 3 in the silica raw material is not less than 0.001 mass%.
- the low silica raw material content than 0.001 wt% of Fe 2 O 3 is a difficult to obtain, also on the content of the Fe 2 O 3 to produce a lower silica material than 0.001 mass% Special processing is required and costs are high.
- alumina containing Al 2 O 3 as a main component or limestone containing CaCO 3 as a main component may be contained in the glass raw material together with the silica raw material.
- Alumina or limestone contains a small amount of iron oxide as an impurity.
- the content of Fe 2 O 3 in the silica raw material exceeds 0.028 mass%, the content of Fe 2 O 3 contained in the molten glass, together with a glass raw material containing other iron oxides, fining of the molten glass In some cases, the value of Fe 2 O 3 content at which the effect is rapidly improved may be exceeded. In this case, the transmittance at a wavelength of 300 nm is adjusted to 30% or more, preferably 40% or more, more preferably 50% or more. May be difficult. Therefore, the content of Fe 2 O 3 in the silica raw material to 0.028 mass% or less.
- the content of Fe 2 O 3 contained in the glass substrate derived from the impurities of the silica raw material is 50% by mass or less with respect to the content of Fe 2 O 3 contained in the glass substrate to be produced. It is preferable.
- oxidation is performed. The clarification effect is demonstrated using the adjustment raw material containing iron, and the freedom degree of adjustment mixing for improving the transmittance
- the glass raw material contains at least limestone as a CaO raw material in addition to the silica raw material.
- the iron oxide contained in the limestone is represented by Fe 2 O 3 and the limestone contains 0.001 to 0.05 mass% of Fe 2 O 3 , it is used as a glass raw material.
- the content of Fe 2 O 3 in the silica raw material is preferably 0.001 to 0.015% by mass.
- the content of Fe 2 O 3 contained in the glass substrate derived from the silica raw material and limestone impurities is 50% by mass or less with respect to the content of Fe 2 O 3 contained in the glass substrate to be produced. More preferably.
- the glass raw material includes at least limestone as a CaO raw material in addition to the silica raw material.
- this limestone contains iron oxide as an impurity
- the iron oxide contained in the limestone is represented by Fe 2 O 3 and the limestone contains 0.001 to 0.05 mass% of Fe 2 O 3 , it is used as a glass raw material.
- the content of Fe 2 O 3 in the silica raw material is preferably 0.001 to 0.0125% by mass.
- the content of Fe 2 O 3 contained in the glass substrate derived from the silica raw material and limestone impurities is 50% by mass or less with respect to the content of Fe 2 O 3 contained in the glass substrate to be produced. More preferably.
- the glass raw material is heated in a melting furnace (not shown) to produce molten glass.
- a clarification process is performed (step S20).
- the molten glass is removed in a clarification tank (not shown) using the above-described clarifier.
- the molten glass in the clarification tank is heated, so that bubbles containing O 2 , CO 2 , SO 2, etc. contained in the molten glass are reduced to Fe 2 O 3 as a clarifier. It grows by absorbing O 2 produced by the reaction, floats on the liquid surface of the molten glass, and is released (defoaming step).
- the temperature of the molten glass is lowered, whereby the oxidation of FeO obtained by the reduction reaction of Fe 2 O 3 which is the clarification agent causes O in the bubbles remaining in the molten glass. 2 is absorbed into the molten glass and the bubbles disappear (absorption process).
- the oxidation reaction and reduction reaction by the fining agent are performed by controlling the temperature of the molten glass.
- SnO 2 is a component to facilitate devitrification glass, since the amount of use is restricted, the content of Fe 2 O 3 Adjustment is preferable in that the clarification effect is effectively controlled.
- step S30 a stirring process is performed (step S30).
- the molten glass is passed through a vertically-shown stirring tank (not shown) in order to maintain chemical and thermal uniformity of the glass. While the molten glass is being stirred by the stirrer provided in the stirring tank, the molten glass moves to the bottom in the vertical downward direction, and is led to a subsequent process. Thereby, nonuniformity of the glass such as striae can be improved.
- a molding process is performed (step S40).
- the method for producing a glass plate there is no particular limitation on the method for producing a glass plate, and a float method or a downdraw method is used.
- the down draw method including overflow down draw, slot down draw, and the like is a known method described in, for example, Japanese Patent Application Laid-Open No. 2010-189220, Japanese Patent No. 3586142, and the like. Thereby, a sheet-like glass ribbon having a predetermined thickness and width is formed.
- an overflow downdraw is most preferable among the downdraw methods, but a slot downdraw may be used.
- a slow cooling process is performed (step S50). Specifically, the glass ribbon formed into a sheet shape is cooled below the annealing point in an annealing furnace (not shown).
- a plate-making process is performed (step S60). Specifically, a continuously produced glass ribbon is sampled at a certain length to obtain a glass plate.
- a shape processing step is performed (step S70). In the shape processing step, the glass end face is ground and polished in addition to cutting into a predetermined glass plate size and shape.
- step S80 an inspection process is performed (step S80).
- the occurrence frequency of defects due to bubbles in the glass substrate is examined, and whether or not the occurrence frequency is a predetermined frequency or less is examined for a predetermined number of glass substrates. That is, it is determined whether or not the glass substrate satisfies the bubble quality (step S90).
- step S90 a blending ratio for increasing the content of Fe 2 O 3 in the molten glass by using an adjustment raw material containing iron oxide or the like Adjustment is performed (step S100), and steps S5 to S90 are repeated again.
- steps S5 to S100 are repeatedly performed until the glass substrate satisfies the bubble quality. However, even if the bubble homogeneity is satisfied once, if the glass substrate is being manufactured, the flow of the above manufacturing method ( Steps S5 to S100) may be performed.
- FIG. 2 shows the spectral transmittance of the glass substrate.
- a plurality of curves show the spectral transmittance which varies depending on the blending adjustment of the raw materials.
- FIG. 2 it can be seen that the transmittance suddenly rises at a wavelength of 250 to 400 nm, and the transmittance at a wavelength of 300 nm varies greatly due to a subtle compositional change of the raw material.
- FIG. 3 is a graph showing an example of transmittance at a wavelength of 300 nm.
- the content of Fe 2 O 3 in the glass substrate is 0.045% by mass or less (450 ppm or less).
- iron oxide contained as an impurity in the silica raw material is Fe 2 O 3 .
- the content of Fe 2 O 3 is expressed at least 0.028 mass% (280 ppm) or less, the content of Fe 2 O 3 contained in the glass substrate derived from the impurities contained in the silica raw material
- the content of Fe 2 O 3 can be made lower than 0.02 mass% to 0.03% by mass (200 to 300 ppm), which is a sharp improvement in the fining effect.
- the total content of Fe 2 O 3 contained in the glass substrate derived from the iron oxide contained in the other raw materials used as the glass raw material can be made lower than 0.02 mass% to 0.03 mass% (200 to 300 ppm), which is the content ratio of Fe 2 O 3 in which the clarification effect is rapidly improved.
- the content of 0.028% by mass of Fe 2 O 3 in the silica raw material does not include a raw material containing iron oxide such as alumina or limestone at the stage before adjusting and blending the glass raw material according to the refining effect. Alternatively, it is an upper limit value assuming that these raw materials contain no iron oxide as an impurity.
- the glass raw material When a glass substrate containing 1 to 10% by mass of CaO is manufactured, the glass raw material includes limestone as a CaO raw material in addition to the silica raw material.
- this limestone contains iron oxide as an impurity, the iron oxide contained in the limestone is represented by Fe 2 O 3 and the limestone contains 0.001 to 0.05 mass% of Fe 2 O 3 , it is used as a glass raw material.
- the content of Fe 2 O 3 in the silica raw material is preferably 0.001 to 0.015% by mass.
- the raw material preparation of the glass raw material is adjusted so that the ultraviolet ray transmittance in the glass substrate becomes 30% or more by using the adjustment raw material containing iron oxide according to the fining effect.
- transmittance at a wavelength of 300 nm is 30% or more, preferably transmittance is 40% or more, more preferably 50% or more Can be performed efficiently.
- the content of Fe 2 O 3 immediately after the clarification effect is dramatically improved can be easily found. Therefore, by maintaining the raw material preparation at this time, a glass substrate having a high ultraviolet transmittance, for example, a transmittance of 40% or more or 50% or more can be stably produced.
- the content of Fe 2 O 3 in the silica raw material is preferably 0.02% by mass (200 ppm) or less, more preferably 0.015% by mass (150 ppm) or less.
- the lower limit of the content of Fe 2 O 3 in the silica starting material is preferably 0.001 mass% (10 ppm). That is, by making the content of Fe 2 O 3 in the silica raw material in the above range, it is possible to efficiently adjust the transmittance of ultraviolet rays and the clarification effect, and to efficiently produce a glass substrate having a preferable transmittance.
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Abstract
Description
液晶パネルを製造する工程においては、ガラス基板を通して紫外線(波長300~380nm)を照射することが行われる。例えば、ガラス基板を通して紫外線(波長300~380nm)を照射して、リソグラフィや、紫外線硬化樹脂による基板の周囲の封止が行われる。また、ガラス基板を通して、紫外線を照射して、液晶材料中の光重合ポリマを重合し、液晶分子の配向を安定化させる方法も用いられる。近年では、波長300~380nmのうち、波長300nm近傍の紫外線が用いられることが多くなり、特に波長300nm近傍の紫外線透過率を向上させることが望まれる。
SiO2を主成分とするシリカ原料と、酸化鉄を含む調整原料とを少なくとも用いて調合してガラス原料をつくる原料調合工程と、
前記ガラス原料を熔解し熔融ガラスとする熔解工程と、
前記熔融ガラスの清澄を行う清澄工程と、を有する。
前記シリカ原料は、不純物として酸化鉄を含み、前記酸化鉄をFe2O3で表したとき、前記シリカ原料は、Fe2O3を0.001~0.028質量%含み、前記調整原料の前記ガラス原料における含有量は、前記液晶表示装置用ガラス基板における波長300nmの透過率が30%以上となるように調整されている。
その際、前記シリカ原料の不純物を由来としてガラス基板に含有されるFe2O3の含有量は、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下である、ことが好ましい。
前記ガラス原料は、前記シリカ原料の他に、前記CaOの原料となる石灰石を含み、
前記石灰石は、酸化鉄を不純物として含み、前記石灰石に含まれる酸化鉄をFe2O3で表したとき、前記石灰石は、Fe2O3を0.001~0.05質量%含むとき、
前記ガラス原料に用いる前記シリカ原料は、Fe2O3を0.001~0.015質量%含む、ことが好ましい。
また、前記ガラス基板は、CaOを1~15質量%を含み、
前記ガラス原料は、前記シリカ原料の他に、前記CaOの原料となる石灰石を含み、
前記石灰石は、酸化鉄を不純物として含み、前記石灰石に含まれる酸化鉄をFe2O3で表したとき、前記石灰石は、Fe2O3を0.001~0.05質量%含むとき、
前記ガラス原料に用いる前記シリカ原料は、Fe2O3を0.001~0.0125質量%含む、ことが好ましい。
前記ガラス基板は、SnO2を0.15~0.25質量%含む、ことが好ましい。
また、製造されるガラス基板に含まれるβ-OH値が0.45/mm以下である、ことが好ましい。
前記ガラス基板はAs2O3及びSb2O3を実質的に含まない、ことが好ましい。
SiO2を主成分とするシリカ原料を少なくとも含むガラス原料を調合する原料調合工程と、
前記ガラス原料を熔解し、熔融ガラスとする熔解工程と、
前記熔融ガラスの清澄を行う清澄工程と、を有する。
前記シリカ原料は、不純物として酸化鉄を含み、前記酸化鉄をFe2O3で表したとき、前記シリカ原料は、Fe2O3を0.001~0.028質量%含む。前記清澄工程における前記熔融ガラスの清澄効果に応じて、前記原料調合工程において、酸化鉄を含む調整原料を用いて、前記ガラス原料を調合する。
SiO2を主成分とし酸化鉄を不純物として含むシリカ原料と、酸化鉄を主成分として含む調整原料とを少なくとも用いて調合してガラス原料をつくる原料調合工程と、
前記ガラス原料を熔解し、熔融ガラスとする熔解工程と、
前記熔融ガラスの清澄を行う清澄工程と、を有する。
前記シリカ原料が不純物として含む前記酸化鉄をFe2O3で表したとき、前記シリカ原料は、該Fe2O3を0.001~0.028質量%含む。
ガラス基板は、SiO2を50~70質量%含有する液晶表示装置用ガラス基板であり、液晶パネルの液晶材料を挟む2枚のガラス基板に用いられる。ガラス基板の厚さは、例えば0.3~0.7mmであり、サイズが300×400mm~2200×2500mmである。また、ガラス基板の透過率は、300nmの波長において30%以上となっている。ここで、300nmの波長の透過率が30%以上であるとは、ガラス基板の厚さが0.3~0.7mmの範囲において、厚さに関係なく300nmの波長の透過率が30%以上であることをいう。ガラス基板の透過率が上記値に設定されるのは、液晶パネルの製造段階で、波長300nmを含む紫外線を照射して行う処理、例えば液晶材料中の光重合ポリマを重合し、液晶分子の配向を安定化させる処理を効率よく行うためである。
また、ガラス基板のβ-OH値は0.45/mm以下であることが好ましい。β-OH値が0.45/mmを越えると、ガラス基板中に発生する気泡による欠陥の発生頻度が高くなる。
SiO2:50~70%(55~68%,58~62%) 、
Al2O3:10~25%(15~20%,15~18%)、
B2O3:4~18%(6~14%,10~13%)、
MgO:0~10%(0~5%,1~2%)、
CaO:0~20%(1~10%,4~7%)、
SrO:0~20%(0~10%,1~3%)、
BaO:0~10%(0~2%,0~1%)、
K2O:0~2%(0.1~2%,0.1~0.5%)、
SnO2:0~1%(0.01~0.5%,0.05~0.4%,0.1~0.3%,0.15~0.25%)、
Fe2O3:0.01~0.045%(0.015~0.04%,0.02~0.035%)。
SiO2:50~70%(55~68%,58~63%) 、
Al2O3:8~25%(10~23%,14~23%)、
B2O3:3~15%(5~15%,6~13%)、
MgO:0~10%(0~7%,0~1%)、
CaO:0~20%(4~14%,5~12%)、
SrO:0~20%(0~10%,0~1%)、
BaO:0~10%(0~2%,0~1%)、
K2O:0~2%(0.1~2%,0.1~0.5%)、
SnO2:0~1%(0.01~0.5%,0.05~0.4%,0.1~0.3%,0.15~0.25%)、
Fe2O3:0.01~0.045%(0.015~0.04%,0.02~0.035%)。
なお、ガラス基板にSnO2を0.15~0.25質量%含ませ、かつ、上記シリカ原料を用いることにより、ガラスの清澄を十分に行うと共に、波長300nmにおける透過率が30%以上となるガラス基板を効率よく製造することができる。
また、β-OH値は、IR分光分析法により測定されるガラス中のヒドロキシル基含有量の尺度であり、ガラス中の水分の尺度となる。β-OH値は、下記式にしたがって求められる。
β-OH値 = (1/W)LOG10(T1/T2)
ここで、Wは試料の厚さ(mm)である。波長2500nm~3000nmの透過率を測定したときに、最大透過率がT1であり、最小透過率がT2である。例えば、T1における波長は、2600nmであり、T2における波長は2800nmである。
SiO2はガラス基板のガラスの骨格をなす成分であり、ガラスの化学的耐久性と耐熱性を高める効果を有している。SiO2含有率が低すぎる場合には化学的耐久性と耐熱性の効果が十分に得られず、SiO2含有率が高すぎるとガラスが失透を起こしやすくなり、成形が困難になるとともに、粘性が上昇してガラスの清澄および均質化が困難になる。
このような原料の中で、ガラス基板中の含有率が最も高いSiO2の原料であるシリカ原料における酸化鉄の含有率を抑制することで、ガラス基板の性質(化学的耐久性、耐熱性、耐酸性、耐失透性、熔融ガラスの粘性等)を維持したまま、後述する清澄工程における清澄効果を容易に制御することができ、波長300nmにおいて30%以上の透過率を有するガラス基板を効率よく製造することができる。
具体的には、シリカ原料における酸化鉄をFe2O3で表したときの含有率(以降、単に、シリカ原料におけるFe2O3の含有率、という)を低く抑えることにより、熔融ガラス中のFe2O3の含有率を、熔融ガラスの清澄効果が急激に向上するFe2O3の含有率の数値以下に予め低く抑え、このとき製造されるガラス基板の気泡による欠陥の発生頻度の判定結果(清澄効果)に応じて、熔融ガラス中のFe2O3の含有率を高くするように、酸化鉄を含む原料を調整原料としてガラス原料の配合調整をする。しかし、欠陥の発生頻度を低くするために熔融ガラス中のFe2O3の含有率を高くすると、波長300nmにおける透過率が低下するので、配合調整するために用いる上記調整原料を必要以上にガラス原料に含ませることはできない。すなわち、配合調整するための調整原料の配合量は、波長300nm近傍における透過率は30%以上となるように制限される。配合調整するための調整原料は、例えば、Fe2O3を主成分(95質量%以上を含む成分)とする酸化第2鉄(ベンガラ)が゛挙げられる。勿論、配合調整前のガラス原料に、シリカ原料のほかに、アルミナ、石灰石等の酸化鉄を不純物として含む原料を含ませることができる。この場合においても、熔融ガラス中の酸化鉄の含有率を、熔融ガラスの清澄効果が急激に向上するFe2O3の含有率の数値以下に予め低く抑えておく。
このように、ガラス基板製造時の熔融ガラスの清澄効果に応じて酸化鉄を含む原料(調整原料)を、シリカ原料、さらには、アルミナあるいは石灰石等の原料を含むガラス原料に付加して配合調整する。これにより、気泡による欠陥の発生頻度がほとんどなく、波長300nm近傍における透過率が高く調整されたガラス基板を効率よく製造することができる。
ガラス基板の製造方法について、まず概要を説明すると、ガラス基板は、ガラス原料の配合調整が行われた段階では、SiO2を主成分とするシリカ原料と、酸化鉄を含む調整原料とを他の原料とともに調合してガラス原料をつくる。このガラス原料を熔解し、熔融ガラスとする。この後、熔融ガラスの清澄を行う。このとき、シリカ原料は酸化鉄を含む。この酸化鉄をFe2O3で表したとき、シリカ原料はFe2O3を不純物として0.028質量%以下含む。また、ガラス原料に含まれる調整原料のガラス原料における含有量は、紫外線の透過率が30%以上となるように調整されている。このような調整原料の含有量は、以下で説明するように、熔融ガラス中のFe2O3の含有率が、清澄効果が急激に向上するFe2O3の含有率の数値をわずかに超えるように、調整される。これにより、波長300nmの透過率が30%以上となるように調整され得る。したがって、Fe2O3の含有率が、熔融ガラス中のFe2O3による清澄効果が急激に向上するときのFe2O3の含有率の値をわずかに越えるために要する調整原料の配合調整量を見出すことが必要になる。一方、この熔融ガラス中のFe2O3による清澄効果が急激に向上するときのFe2O3の含有率の値は、ガラス基板の組成によって変動する。また、ガラス基板の製造条件やガラス基板の組成の微妙な変動等によっても変動する。よって、上記配合調整量を予め見出すことは難しい。このため、以下に説明するように、上記調整原料の配合調整量を見出すことができるように、シリカ原料はFe2O3を不純物として0.028質量%(酸化鉄をFe2O3で表したときの含有率)以下含むようにする。これにより、熔融ガラス中に含まれるシリカ原料に由来するFe2O3の含有率を、熔融ガラス中のFe2O3による清澄効果が急激に向上するときの上記Fe2O3の含有率の値より低くすることができる。
この他に、Al2O3を主成分とするアルミナ、あるいはCaCO3を主成分とする石灰石等がシリカ原料とともにガラス原料に含まれていてもよい。アルミナ、あるいは石灰石には、微量の酸化鉄が不純物として含まれている。シリカ原料におけるFe2O3の含有率が0.028質量%を越えると、熔融ガラスに含まれるFe2O3の含有率が、他の酸化鉄を含むガラス原料とあいまって、熔融ガラスの清澄効果が急激に向上するFe2O3の含有率の数値を超える場合があり、この場合、波長300nmにおける透過率を30%以上、好ましくは40%以上、より好ましくは50%以上に調整することはでき難い場合がある。このため、シリカ原料におけるFe2O3の含有率を0.028質量%以下とする。このとき、シリカ原料の不純物を由来としてガラス基板に含有されるFe2O3の含有量は、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下である、ことが好ましい。シリカ原料の不純物を由来としてガラス基板に含有されるFe2O3の含有量を、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下とすることにより、酸化鉄を含む調整原料を用いて清澄効果を発揮させ、かつ紫外線の透過率が向上するための調整配合の自由度を確保することができる。しかも、清澄効果を確保しつつ、Fe2O3の含有率を抑制することができるので、より紫外線の高い透過率を有するガラス基板を製造することができる。
また、CaOを1~10質量%を含むガラス基板を製造する場合、ガラス原料は、シリカ原料のほか、CaOの原料となる石灰石を少なくとも含む。この石灰石が、酸化鉄を不純物として含み、石灰石に含まれる酸化鉄をFe2O3で表して、石灰石がFe2O3を、0.001~0.05質量%含むとき、ガラス原料に用いるシリカ原料におけるFe2O3の含有率は0.001~0.015質量%であることが好ましい。このとき、シリカ原料および石灰石の不純物を由来としてガラス基板に含有されるFe2O3の含有量は、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下である、ことがより好ましい。
また、CaOを1~15質量%を含むガラス基板を製造する場合、ガラス原料は、シリカ原料のほか、CaOの原料となる石灰石を少なくとも含む。この石灰石が、酸化鉄を不純物として含み、石灰石に含まれる酸化鉄をFe2O3で表して、石灰石がFe2O3を、0.001~0.05質量%含むとき、ガラス原料に用いるシリカ原料におけるFe2O3の含有率は0.001~0.0125質量%であることが好ましい。このとき、シリカ原料および石灰石の不純物を由来としてガラス基板に含有されるFe2O3の含有量は、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下である、ことがより好ましい。
次に、熔解工程(ステップS10)では、図示されない熔解炉で、ガラス原料が加熱されて熔融ガラスが作られる。
Fe2O3の他に、SnO2等も清澄剤として機能するが、SnO2は、ガラスを失透し易くする成分であり、使用量が制限されるため、Fe2O3の含有率を調整することが、清澄効果を効果的に制御する点で好ましい。
次に、採板工程が行われる(ステップS60)。具体的に、連続的に生産されるガラスリボンは一定の長さ毎に採板されガラス板が得られる。
この後、形状加工工程が行われる(ステップS70)。形状加工工程では、所定のガラス板のサイズや形状に切り出す他、ガラス端面の研削・研磨が行われる。
また、CaOを1~10質量%を含むガラス基板を製造する場合、ガラス原料は、シリカ原料のほか、CaOの原料となる石灰石を含む。この石灰石が、酸化鉄を不純物として含み、石灰石に含まれる酸化鉄をFe2O3で表して、石灰石がFe2O3を、0.001~0.05質量%含むとき、ガラス原料に用いるシリカ原料におけるFe2O3の含有率は0.001~0.015質量%であることが好ましい。
このように、シリカ原料と調整原料を用いて原料調合をする前の段階では、熔融ガラスに含まれるFe2O3の含有率を、Fe2O3による清澄効果が急激に向上するFe2O3の含有率の値より低く抑えることができるので、清澄効果に応じて、酸化鉄を含む調整原料を用いて、ガラス基板における紫外線透過率が30%以上となるように、ガラス原料の原料調合をすることができ、気泡による欠陥が基準値以下であり、波長300nmの透過率が30%以上であって、好ましくは透過率が40%以上、より好ましくは50%以上であるガラス基板の製造を効率よく行うことができる。特に、本実施形態では、清澄効果が劇的に向上する直後のFe2O3の含有率を容易に見出すことができる。したがって、このときの原料調合を維持することにより、紫外線の高い透過率、例えば、40%以上あるいは50%以上の透過率を有するガラス基板を安定的に製造することができる。
シリカ原料におけるFe2O3の含有率は、好ましくは0.02質量%(200ppm)以下であり、より好ましくは0.015質量%(150ppm)以下である。シリカ原料におけるFe2O3の含有率の下限は好ましくは0.001質量%(10ppm)である。すなわち、シリカ原料におけるFe2O3の含有率を上記範囲にすることで、紫外線の透過率と清澄効果を効率よく調整して、好ましい透過率を有するガラス基板を効率よく製造することができる。
Claims (11)
- SiO2およびFe2O3を含有し、SiO2の含有率が50~70質量%である液晶表示装置用ガラス基板の製造方法であって、
SiO2を主成分とするシリカ原料と、酸化鉄を含む調整原料とを少なくとも用いて調合してガラス原料をつくる原料調合工程と、
前記ガラス原料を熔解し熔融ガラスとする熔解工程と、
前記熔融ガラスの清澄を行う清澄工程と、を有し、
前記シリカ原料は、不純物として酸化鉄を含み、前記酸化鉄をFe2O3で表したとき、前記シリカ原料は、Fe2O3を0.001~0.028質量%含み、前記調整原料の前記ガラス原料における含有量は、前記液晶表示装置用ガラス基板における波長300nmの透過率が30%以上となるように調整されている、ことを特徴とするガラス基板の製造方法。 - 前記調整原料の前記含有量は、さらに、前記熔融ガラスの前記清澄工程における清澄効果に応じて調整されている、請求項1に記載のガラス基板の製造方法。
- 前記シリカ原料の不純物を由来としてガラス基板に含有されるFe2O3の含有量は、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下である、請求項1または2に記載のガラス基板の製造方法。
- 前記ガラス基板は、CaOを1~10質量%を含み、
前記ガラス原料は、前記シリカ原料の他に、前記CaOの原料となる石灰石を含み、
前記石灰石は、酸化鉄を不純物として含み、前記石灰石に含まれる酸化鉄をFe2O3で表したとき、前記石灰石は、Fe2O3を0.001~0.05質量%含むとき、
前記ガラス原料に用いる前記シリカ原料は、Fe2O3を0.001~0.015質量%含む、請求項1~3のいずれか1項に記載のガラス基板の製造方法。 - 前記ガラス基板は、CaOを1~15質量%を含み、
前記ガラス原料は、前記シリカ原料の他に、前記CaOの原料となる石灰石を含み、
前記石灰石は、酸化鉄を不純物として含み、前記石灰石に含まれる酸化鉄をFe2O3で表したとき、前記石灰石がFe2O3を0.001~0.05質量%含むとき、
前記ガラス原料に用いる前記シリカ原料は、Fe2O3を0.001~0.0125質量%含む、請求項1~3のいずれか1項に記載のガラス基板の製造方法。 - 前記シリカ原料および前記石灰石の不純物を由来としてガラス基板に含有されるFe2O3の含有量は、製造されるガラス基板に含まれるFe2O3の含有量に対して50質量%以下である、請求項4または5に記載のガラス基板の製造方法。
- 前記ガラス基板は、SnO2を0.15~0.25質量%含む、請求項1~6のいずれか1項に記載のガラス基板の製造方法。
- 製造されるガラス基板のβ-OH値が0.45/mm以下である、請求項1~7のいずれか1項に記載のガラス基板の製造方法。
- 前記ガラス基板にAs2O3及びSb2O3を実質的に含まない、請求項1~8のいずれか1項に記載のガラス製造方法。
- SiO2およびFe2O3を含有し、SiO2の含有率が50~70質量%である液晶表示装置用ガラス基板の製造方法であって、
SiO2を主成分とするシリカ原料を少なくとも含むガラス原料を調合する原料調合工程と、
前記ガラス原料を熔解し熔融ガラスとする熔解工程と、
前記熔融ガラスの清澄を行う清澄工程と、を有し、
前記シリカ原料は、不純物として酸化鉄を含み、前記酸化鉄をFe2O3で表したとき、前記シリカ原料は、Fe2O3を0.001~0.028質量%以下含み、前記清澄工程における前記熔融ガラスの清澄効果に応じて、前記原料調合工程において、酸化鉄を含む調整原料を用いて、前記ガラス原料を調合することを特徴とするガラス基板の製造方法。 - SiO2およびFe2O3を含有し、SiO2の含有率が50~70質量%であり、波長300nmの紫外線透過率が30%以上である液晶表示装置用ガラス基板の製造方法であって、
SiO2を主成分とし酸化鉄を不純物として含むシリカ原料と、酸化鉄を主成分として含む調整原料とを少なくとも用いて調合してガラス原料をつくる原料調合工程と、
前記ガラス原料を熔解し熔融ガラスを生成する熔解工程と、
生成した熔融ガラスの清澄を行う清澄工程と、を有し、
前記シリカ原料が不純物として含む前記酸化鉄をFe2O3で表したとき、前記シリカ原料は、該Fe2O3を0.001~0.028質量%含む、ことを特徴とするガラス基板の製造方法。
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