CN105621883A - Liquid crystal substrate glass and preparation method thereof - Google Patents
Liquid crystal substrate glass and preparation method thereof Download PDFInfo
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- CN105621883A CN105621883A CN201610079878.8A CN201610079878A CN105621883A CN 105621883 A CN105621883 A CN 105621883A CN 201610079878 A CN201610079878 A CN 201610079878A CN 105621883 A CN105621883 A CN 105621883A
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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
- C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
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Abstract
The invention discloses liquid crystal substrate glass and a preparation method thereof. The liquid crystal substrate glass comprises, by mass, 54-70% of SiO2, 13-18% of Al2O3, 9-12% of B2O, 0.5-2% of MgO, 6-10% of CaO, 1.05-3% of SrO, 0.2-1% of BaO, 0.01-0.5% of K2O, 0.016-0.059% of Na2O, 0.002-2% of ZnO, 0.16-0.3% of SnO2, 0.02-0.05% of Zr and 0.001-0.01% of Fe2O3. By studying ingredients of the liquid crystal substrate glass and adjusting composition of the ingredients, devitrification temperature interval is lowered, a retention layer of the glass is eliminated, and devitrification of a forming area can be improved.
Description
Technical field
The invention belongs to liquid crystal substrate glass technical field, be specifically related to a kind of liquid crystal substrate glass and preparation method thereof.
Background technology
LCD glass substrate (GlassSubstrate) refers to liquid crystal display glass substrate, and one piece of liquid crystal panel needs two panels glass substrate, wherein a piece of is used in colored filter, a piece of is used in above transparency electrode.
When preparing TFT-LCD panel, a surface at glass substrate is needed to make various films, circuit and figure, first have to form nesa coating, dielectric film, quasiconductor (polysilicon, unformed silicon etc.) film and metal film by technology such as sputtering, chemical gaseous phase depositions (CVD) on base plate glass surface, then pass through optical lithography and form various circuit and figure. In film deposition and photoetch stage, glass substrate to stand various heat treatment and chemical action, and wherein the forming process of semiconductor film to stand 500��600 DEG C of high-temperature process. Usually, the glass as TFT type liquid crystal display substrate should meet following Property requirements:
Being substantially free of alkali metal oxide in glass, in high-temperature process, alkali metal ion can be diffused into semiconductor film, the performance of infringement semiconductor film.
Owing to base plate glass need to clean and etching through a large amount of reagent, for avoiding the precipitation of composition in glass, glass must have high chemical stability, particularly has strong acid and alkali resistance performance.
Glass has the coefficient of expansion matched with polysilicon and amorphous silicon material, and its optimum is (25��40) �� 10-7/ DEG C, difference therebetween is generally not to be exceeded 20%.
Glass has relatively low density, especially for large scale flat faced display, it is desirable to alleviate the weight of glass substrate as far as possible.
For large-scale LCD glass substrate, thickness substrate area when 0.7mm or 0.5mm reaches 1��2, or bigger size. For preventing sheets of glass in transport, the course of processing owing to gravity causes glass sag deformation and crushes, it is necessary to improve the bending strength of glass substrate, make base plate glass be subject to when external force or self gravitation and do not deform upon or less deformation occurs.
Additionally, constantly develop to directions such as large scale, fine definition, high brightness to adapt to liquid crystal display, more excellent in performance is proposed TFT-LCD liquid crystal substrate glass.
Owing to the display of LCD adopts " back transmission " radiation modality, the utilization rate of backlight luminescence is subject to the organic dyestuff impacts such as liquid crystal material angle, color filter plate, the luminous utilization rate of backlight is not high, brightness is significantly not as Display Techniques such as CRT, PDP and OLED, therefore, improve light source utilization rate and be always up, to reach lifting brightness, the direction that liquid crystal display is made great efforts to develop. So, the light transmittance improving liquid crystal substrate glass can better play its effect. Current main flow base plate glass light transmittance reaches 90%, and light transmittance is more high more good.
Except above-mentioned Property requirements, in presentation quality, base plate glass should have sufficiently high degree of homogenization, flatness and non-nuclear density gauge. From the angle of glass smelting and molding, glass also should have fusibility, can not only ensure to produce high-quality, lacks the original sheet glass of defect as far as possible, and glass smelting temperature also should be made unsuitable too high, and too high glass melting temperature will bring difficulty to glass substrate Producer.
Produce in several maturation methods of liquid crystal glass base at present, the most outstanding with the overflow method of forming. Because adopting the base plate glass that the overflow method of forming produces without the surface grinding of rear operation and polishing.
From the requirement of above-mentioned LCD glass substrate it can be seen that LCD substrate is very high to the requirement of glass physical, chemistry and technique. Therefore, in order to meet the above-mentioned glass physical Property requirements must being fulfilled for, it is common to TFT-LCD liquid crystal substrate glass adopt RO-SiO2Al2O3B2O3The silicate glass containing boron and aluminium without alkali of system.
Another difficult problem that TFT-LCD liquid crystal substrate glass produces comes from without owing some requirement. So-called glass is owed point and is referred to bubble, glass knot, platinum grain and calculus etc. The resolution of liquid crystal display is more high, requires more strict for glass plate latent defect. The light that backlight sends must cross the pixel and then formation image that grid is formed one by one. The deficient point that any light tight or obstruction light existed in glass passes through all can affect the perfection of image, the tolerance of deficient spot size size is determined according to elemental area, the highest tolerance limit is single elemental area the 25% of general deficient some area, for instance: a display with 100um Pixel Dimensions allows for 50um size and owes point.
In the production technology of the overflow method of forming, the very crucially elimination to bubble. Historically, the bubble eliminated in glass is generally the use such variable valency metal oxide of arsenic. The low temperature oxygen uptake unique due to arsenic oxide arsenoxide and high temperature put oxygen characteristic, help vitreous humour to discharge bubble in glass clarifying process preferably. But, arsenic oxide arsenoxide itself belongs to severe poisonous chemicals, and operator are high-risk operations by its operation process. In recent years, environment and the problem of healthy aspect that arsenic oxide arsenoxide brings as clarifier were increasingly subject to international attention, therefore, this area is always for manufacturing low arsenic or Arsenic-free glass and effort, it addition, in the fabrication process, devitrification of glass defect is always up the key technology of puzzlement production and quality.
Summary of the invention
It is an object of the invention to provide a kind of liquid crystal substrate glass and preparation method thereof, with the defect overcoming above-mentioned prior art to exist, the present invention is by studying the composition of liquid crystal substrate glass, adjust its composition, recrystallization temperature interval is made to decline, eliminate glass retention layer, it is possible to improve the generation of shaping area crystallize.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that
A kind of liquid crystal substrate glass, in mass fraction, described liquid crystal substrate glass includes:
SiO2: 54��70%; Al2O3: 13��18%; B2O3: 9��12%; MgO:0.5��2%; CaO:6��10%; SrO:1.05��3%; BaO:0.2��1%; K2O:0.01��0.5%; Na2O:0.016��0.059%; ZnO:0.002��2%; SnO2: 0.16��0.3%; Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%.
Further, SiO2Introduced by silica flour, and silica flour particle diameter��0.020mm, purity > 99%.
Further, B2O3Introduced by boric anhydride, and boric anhydride purity >=99.50%.
Further, B2O3Introduced by boric anhydride, Al2O3Being introduced by alumina powder, CaO is introduced by calcium carbonate, and MgO is introduced by magnesium carbonate, and SrO is introduced by strontium nitrate, and BaO is introduced by barium nitrate, and ZnO is introduced by zinc oxide, SnO2Introduced by stannum oxide, K2O is introduced by potash feldspar, and the purity > 99% of alumina powder, calcium carbonate, magnesium carbonate, strontium nitrate, barium nitrate, zinc oxide, stannum oxide and potash feldspar.
Further, the density of described liquid crystal substrate glass is 2.33��2.5g/cm3; Recrystallization temperature is 1137��1220 DEG C; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%.
Further, the air bubble content every kilogram number < of described liquid crystal substrate glass 0.1, bubble size is < 0.1mm.
The preparation method of a kind of liquid crystal substrate glass, comprises the following steps:
(1) weigh frit: silica flour, alumina powder, boric anhydride, magnesium carbonate, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide, make liquid crystal substrate glass include following component, in mass fraction: SiO2: 54��70%; Al2O3: 13��18%; B2O3: 9��12%; MgO:0.5��2%; CaO:6��10%; SrO:1.05��3%; BaO:0.2��1%; K2O:0.01��0.5%; Na2O:0.016��0.059%; ZnO:0.002��2%; SnO2: 0.16��0.3%; Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix, then add mixing system together with remaining frit, after mixing fully, compound is taken in batch can;
(3) compound of income batch can is added tank furnace, manufacture liquid crystal substrate glass according to overflow downdraw.
Further, tank furnace temperature is 1500��1650 DEG C.
Further, air bubble content every kilogram number < 0.1 in the liquid crystal substrate glass prepared, bubble size is < 0.1mm;
The liquid crystal substrate glass density prepared is 2.33��2.5g/cm3; Recrystallization temperature is 1137��1220 DEG C; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%.
Compared with prior art, the present invention has following useful technique effect:
The liquid crystal substrate glass of the present invention, introduces K2O and Na2O; Add K2O and Na2During O, the structure of glass changes, and passes through K2O and Na2The free oxygen that O provides, reduces glass softening point temperature, is ensureing that MgO is under certain proportion simultaneously, is playing reduction devitrification of glass temperature by adjusting CaO, SrO, BaO ratio, and obtained liquid crystal substrate glass density is 2.33��2.5g/cm3; Recrystallization temperature is 1137��1220 DEG C; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%, composition is suitable for producing area liquid crystal substrate glass more than 1.4, the clarification with platinum pipeline is melted by tank furnace, the air bubble content every kilogram number < of product glass 0.1, bubble size is < 0.1mm.
The inventive method, by studying the composition of liquid crystal substrate glass, adjusts its composition, makes recrystallization temperature interval decline, eliminate glass retention layer, it is possible to improving the generation of shaping area crystallize, obtained liquid crystal substrate glass density is 2.33��2.5g/cm3; Recrystallization temperature is 1137��1220 DEG C; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%, composition is suitable for producing area liquid crystal substrate glass more than 1.4, the clarification with platinum pipeline is melted by tank furnace, the air bubble content every kilogram number < of product glass 0.1, bubble size is < 0.1mm.
Accompanying drawing explanation
Fig. 1 present invention tests high-temperature stage microscopy work schematic diagram used.
Wherein, 1, cooling water; 2, sapphire sheet; 3, platinum crucible; 4, heating microscope; 5, glass sample.
Detailed description of the invention
Below embodiments of the present invention are described in further detail:
A kind of liquid crystal substrate glass, it is characterised in that in mass fraction, in described liquid crystal substrate glass, oxide includes: SiO2: 54��70%; Al2O3: 13��18%; B2O3: 9��12%; MgO:0.5��2%; CaO:6��10%; SrO:1.05��3%; BaO:0.2��1%; K2O:0.01��0.5%; Na2O:0.016��0.059%; ZnO:0.002��2%; SnO2: 0.16��0.3%; Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%.
SiO2And Na2O introduces by silica flour, and silica flour particle diameter��0.020mm, purity > 99%; B2O3Introduced by boric anhydride, and boric anhydride purity > 99.50%; B2O3Introduced by boric anhydride, Al2O3Being introduced by alumina powder, CaO is introduced by calcium carbonate, and MgO is introduced by magnesium carbonate, and SrO is introduced by strontium nitrate, and BaO is introduced by barium nitrate, and ZnO is introduced by zinc oxide, SnO2Introduced by stannum oxide, K2O is introduced by potash feldspar, and the purity > 99% of alumina powder, calcium carbonate, magnesium carbonate, strontium nitrate, barium nitrate, zinc oxide, stannum oxide and potash feldspar.
The preparation method of a kind of liquid crystal substrate glass, comprises the following steps:
(1) weigh frit: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide, make oxide in liquid crystal substrate glass include following composition, in mass fraction: SiO2: 54��70%; Al2O3: 13��18%; B2O3: 9��12%; MgO:0.5��2%; CaO:6��10%; SrO:1.05��3%; BaO:0.2��1%; K2O:0.01��0.5%; Na2O:0.016��0.059%; ZnO:0.002��2%; SnO2: 0.16��0.3%; Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%;
(2) take zinc oxide+part silica flour and form mixture, then stannum oxide and mixture are pressed the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1500��1650 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
The density of the liquid crystal substrate glass prepared is 2.33��2.5g/cm3; Elastic modelling quantity is more than 70GPa; Recrystallization temperature is 1137��1220 DEG C; Bending strength is more than 110MPa; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%, and air bubble content every kilogram number < 0.1, bubble size is < 0.1mm.
As the transparent glass substrate of liquid crystal display, use Boroalumino silicate glasses. Glass ingredient with the addition of multiple RO diatomic base slaine to promote the formation of glass network; Meanwhile, introduce trace alkali metal, when adding K2O and Na2After O, the structure of boron changes, and passes through K2O and Na2The free oxygen that O provides, by boron oxygen triangle body [BO3] it is changed into boron oxygen tetrahedron [BO4], make the structure of boron from layer structure to rack-like structural transformation, for B2O3And SiO2The glass forming uniformity creates conditions.
Due to the SiO used in a large number2It is refractory material (SiO2Fusing point 1710 DEG C), and B2O3It is good melting promotor and good network added body, glass ingredient with the addition of B2O3As melting promotor to reduce glass manufacture temperature. The B of appropriate amount2O3SiO can be accelerated2Melting, it is possible to the formation of silicate being reacted and changes to lower temperature region, simultaneously because the reduction of the formation of minimum eutectic, surface tension or viscosity, making batch composition strongly be invaded profit, thus improving homogenization. Due to the addition of melting promotor, not only accelerate the fusing speed of dispensing, reduce glass melting temperature, too increase simultaneously needed for glass fining stage from discrete time, the melting accelerating silica flour has become the key point of clarification quality.
Initial mixture of founding is allow SiO in advance2And B2O3It is dissolved in together, so SiO2Raw material silica flour must be fulfilled for the needs that liquid crystal substrate glass produces, in order to promote to melt, silica flour should have��particle diameter of 0.020mm, purity > 99%; Boric anhydride (B2O3) in fusion processes, experience melts and resolidification, so to the more requirement of particle diameter, but the necessary < 0.05% of impurity content, to prevent from introducing the harmful substance in glass. SiO2Content controls 54��70%, B2O3Content control 9��12%.
The content of aluminium oxide is 13��18%, the Al of high-load2O3Contribute to the improvement of strain point of glass, bending strength, but too high, make the easy crystallize of glass.
RO (R is Mg, Ca, Sr, Ba, Zn) is glass network instrumentality. The kind used is numerous, and the raw material and the amount that introduce RO are as follows:
The raw material introducing CaO is calcium carbonate. Glass structure is acted the effect of gathering by Ca. CaO scalable reduces high temperature viscosity and significantly improves the melting behaviour of glass and do not reduce the strain point of glass, and too much CaO then can reduce glass chemical resistance. In glass ingredient, the content of CaO controls 6��10%.
The raw material introducing MgO is magnesium carbonate. MgO can reduce crystallization tendency and crystallization rate, improves chemical stability and the mechanical strength of glass. But its content should not be too much, the easy crystallize of glass and the coefficient of expansion otherwise can be caused too high. In glass ingredient, the content of MgO controls 0.5��2%.
SrO and BaO is respectively provided with to be increased glass chemical-resistant stability and improves the effect of the anti-crystallize of glass. But substantial amounts of SrO and BaO can cause glass density and the coefficient of expansion to increase. SrO and BaO has to be especially improved glass chemical-resistant component. The raw material introducing SrO is strontium nitrate, and in glass, SrO content controls 1.05��3%; The raw material introducing BaO is barium nitrate, and in glass, BaO content controls 0.2��1%.
ZnO can reduce glass high temperature viscosity, increases the chemical resistance of glass, reduces the thermal coefficient of expansion of glass. But ZnO reduces the strain point of glass when content is too much. In the present invention, the introducing material of ZnO is zinc oxide, and in glass, ZnO content controls 0.002��2%.
SnO2It is the oxide that appraises at the current rate, adds as melting promotor and clarifier in this glass forms. But too much SnO2Glass is easily made to precipitate out undesirable calculus, therefore, SnO2Introduced by stannum oxide, the SnO in glass2Content controls 0.16��0.3%.
Micro amount of oxygen compound in glass, as unavoidably introducing composition in raw material, therefore is also necessary to be controlled by other oxide. Represent by mass percentage: Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%.
Frit can be effectively promoted frit and melt and clarification, and then substitutes arsenic oxide arsenoxide clarifier.
Being suitable for producing area liquid crystal substrate glass more than 1.4, melt the clarification with platinum pipeline by tank furnace, the air bubble content every kilogram number < of product glass 0.1, bubble size is < 0.1mm.
For TFT-LCD base plate glass production technology, manufacturing process commonly used at present is overflow downdraw, and for overflow forming process, most stringent of requirement is the high temperature viscosity of the liquidus temperature TL (LiquidusTemperature) of glass and glass, because it is low that overflow downdraw draws the load of vitreous humour during sheets of glass, the flowing of vitreous humour is slower, can not quickly cool down as float glass processes and shape, so the pull at TFT-LCD base plate glass thin plate shapes viscosity 104��1011.5Within the scope of dPa s, any crystallize can not be had under vitreous humour and the Long contact time of refractory material and platinum channel, therefore when designing the chemical composition of base plate glass, the crystallize ceiling temperature reducing glass should be considered as far as possible, reduce the crystalline range of glass, that is allow the liquidus temperature of glass as much as possible lower than the forming temperature of vitreous humour, and the recrystallization temperature upper limit of glass will as far as possible lower than the liquidus temperature of glass, thus can avoid in overflow channel forming process, producing crystallize at TFT-LCD base plate glass, especially glass melt is avoided during the cooling of glass corbel back slab, crystallize to occur in overflow downdraw process.
The liquidus temperature of glass is exactly balance the maximum temperature coexisted between melten glass and primary phase, and the liquidus temperature of glass depends primarily on the chemical composition of glass, is that the method disappeared to precipitate out crystal melt in glass part crystallize sample measures.
The liquidus temperature of glass is difficult to assessment when current experimental technique, the highest recrystallization temperature of general glass is as the liquidus temperature of glass, and the viscosity corresponding on characteristic temperature-viscograph with the highest recrystallization temperature, namely think the viscosity that the liquidus temperature of glass is corresponding, assess whether glass meets the requirement that overflow downdraw shapes with this.
The method of testing of the crystallization property of conventional glass is gradient oven process, but the experimental period of gradient oven process is very long, experimentation complexity is loaded down with trivial details, first have to glass sample is incubated 24 hours in thermal gradient furnace, then at high temperature quickly remove, cool down rapidly in atmosphere, after glass sample cools down, again glass sample is first cut into thin slice, it is then passed through corase grind, finishing polish again after fine grinding, then the degree of crystallization of sight glass whether crystallize and glass under 200 times of optical microscopes, the temperature range scope of the recrystallization temperature of gradient oven process tested glass is very wide, and can not make for the recrystallization temperature of glass and judging accurately.
The method of testing of the devitrification of glass performance used by the present invention is heating microscope method, adopts the heating microscope method (HotStageMicroscopy) can the direct crystallize crystal morphology of sight glass can accurately test out the recrystallization temperature of glass. The temperature measuring device of experiment test devitrification of glass temperature is cold and hot of Britain LinkamTHMSG600, the temperature of cold and hot carrys out regulable control by a set of survey temperature-controlling system, for regulating the temperature of testboard in temp measuring system, it is illustrated in figure 1 high-temperature stage microscopy work schematic diagram.
The principle of the recrystallization temperature of heating microscope method tested glass is first to select to load in platinum crucible 3 after the glass sample 5 grinding finishing polish is cleaned, dried without any glass defect (such as bubble, calculus and striped etc.) and surface to be placed in the sapphire sheet 2 in the micro furnace of high-temperature stage, for the thermocouple of test thermal station temperature under sapphire sheet 2, then design temperature program, micro furnace is warming up to 1450 DEG C makes glass sample 5 melt, and it is incubated half an hour to get rid of the bubble of glass surface, then again glass sample 5 is progressively cooled to close to room temperature, because glass sample 5 is subject to the heat effect of thermal source, by the thermal conductance process of glass, the bottom temp of glass sample 5 is higher compared with the upper surface temperature of glass sample Yu air contact, this upper and lower surface temperature difference just because of glass sample, glass is made namely to form the thermograde of inside glass in thermal conductance process, then pass through utilization cooling water 1 and reduce the temperature of the air contacted with glass top surface to reduce the upper surface temperature of glass, this ensures that there the crystallize layer being carried out sight glass upper surface by heating microscope 4, heating makes the nucleus in glass be formed and grow up again, when temperature rises towards the liquidus temperature of glass, it is seen that the crystal in glass starts melted tailing off, heat up 5 DEG C every time, and be incubated 5 minutes, until all of crystallize crystal melts, last temperature is the crystallize ceiling temperature of glass, the i.e. liquidus temperature of glass, utilizes high-temperature stage microscopes to accurately measure the recrystallization temperature of glass sample, adopts repetitive measurement to average for each glass sample.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1500 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 2
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1650 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 3
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1600 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 4
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1570 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 5
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1620 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 6
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1630 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 7
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1590 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Embodiment 8
(1) frit is weighed: silica flour, alumina powder, boric anhydride, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix 20 minutes, then add mixing system together with remaining frit, after being sufficiently mixed 25 minutes, compound is taken in batch can;
(3) compound of income batch can is added the tank furnace that temperature is 1610 DEG C, manufacture liquid crystal substrate glass according to overflow downdraw.
Liquid crystal glass base respectively 1#��8#, the 1# that embodiment 1��embodiment 8 prepares��4# is as shown in table 1, and 5#��8# is as shown in table 2:
The liquid crystal substrate glass sample of table 1 embodiment 1��4 preparation
The liquid crystal substrate glass sample of table 2 embodiment 5��8 preparation
Claims (9)
1. a liquid crystal substrate glass, it is characterised in that in mass fraction, described liquid crystal substrate glass includes:
SiO2: 54��70%; Al2O3: 13��18%; B2O3: 9��12%; MgO:0.5��2%; CaO:6��10%; SrO:1.05��3%; BaO:0.2��1%; K2O:0.01��0.5%; Na2O:0.016��0.059%; ZnO:0.002��2%; SnO2: 0.16��0.3%; Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%.
2. a kind of liquid crystal substrate glass according to claim 1, it is characterised in that SiO2Introduced by silica flour, and silica flour particle diameter��0.020mm, purity > 99%.
3. a kind of liquid crystal substrate glass according to claim 1, it is characterised in that B2O3Introduced by boric anhydride, and boric anhydride purity >=99.50%.
4. a kind of liquid crystal substrate glass according to claim 1, it is characterised in that B2O3Introduced by boric anhydride, Al2O3Being introduced by alumina powder, CaO is introduced by calcium carbonate, and MgO is introduced by magnesium carbonate, and SrO is introduced by strontium nitrate, and BaO is introduced by barium nitrate, and ZnO is introduced by zinc oxide, SnO2Introduced by stannum oxide, K2O is introduced by potash feldspar, and the purity > 99% of alumina powder, calcium carbonate, magnesium carbonate, strontium nitrate, barium nitrate, zinc oxide, stannum oxide and potash feldspar.
5. a kind of liquid crystal substrate glass according to claim 1, it is characterised in that the density of described liquid crystal substrate glass is 2.33��2.5g/cm3; Recrystallization temperature is 1137��1220 DEG C; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%.
6. a kind of liquid crystal substrate glass according to claim 1, it is characterised in that the air bubble content every kilogram number < of described liquid crystal substrate glass 0.1, bubble size is < 0.1mm.
7. the preparation method of a liquid crystal substrate glass, it is characterised in that comprise the following steps:
(1) weigh frit: silica flour, alumina powder, boric anhydride, magnesium carbonate, calcium carbonate, strontium nitrate, barium nitrate, zinc oxide, potash feldspar and stannum oxide, make liquid crystal substrate glass include following component, in mass fraction: SiO2: 54��70%; Al2O3: 13��18%; B2O3: 9��12%; MgO:0.5��2%; CaO:6��10%; SrO:1.05��3%; BaO:0.2��1%; K2O:0.01��0.5%; Na2O:0.016��0.059%; ZnO:0.002��2%; SnO2: 0.16��0.3%; Zr02: 0.02��0.05%; Fe2O3: 0.001��0.01%;
(2) take the mixture of stannum oxide and zinc oxide+part silica flour by the quality of 1:9 than premix, then add mixing system together with remaining frit, after mixing fully, compound is taken in batch can;
(3) compound of income batch can is added tank furnace, manufacture liquid crystal substrate glass according to overflow downdraw.
8. the preparation method of a kind of liquid crystal substrate glass according to claim 7, it is characterised in that tank furnace temperature is 1500��1650 DEG C.
9. the preparation method of a kind of liquid crystal substrate glass according to claim 7, it is characterised in that air bubble content every kilogram number < 0.1 in prepared liquid crystal substrate glass, bubble size is < 0.1mm;
The liquid crystal substrate glass density prepared is 2.33��2.5g/cm3; Recrystallization temperature is 1137��1220 DEG C; Strain point temperature is 665.4��676.1 DEG C; It is (34.8��36.8) �� 10 at the thermal coefficient of expansions of 30��380 DEG C-7/ DEG C; In 500��600nm wavelength, light transmission rate is more than 92%.
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