CN106495468A - A kind of ultra-thin glass of low surface tension and preparation method thereof - Google Patents
A kind of ultra-thin glass of low surface tension and preparation method thereof Download PDFInfo
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- CN106495468A CN106495468A CN201610891402.4A CN201610891402A CN106495468A CN 106495468 A CN106495468 A CN 106495468A CN 201610891402 A CN201610891402 A CN 201610891402A CN 106495468 A CN106495468 A CN 106495468A
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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
-
- 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
-
- 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
- G02F1/133302—Rigid substrates, e.g. inorganic substrates
Abstract
The invention belongs to photoelectric display field, relates generally to a kind of ultra-thin glass as TFT LCD display base plates and preparation method thereof.A kind of ultra-thin glass of low surface tension, it is characterised in that its chemical composition is by weight percentage:SiO258 68wt.%, Al2O316 24wt.%, B2O32 7wt.% of 2 9wt.% of 5 12wt.%, CaO, MgO, 3 13wt.% of SrO, MoO31 4wt.%, V2O50 2wt.%, WO30 3wt.%, SnO20.1 0.2wt.%;Wherein SiO2+Al2O3Scope:The scope of 77 85wt.%, MgO+CaO+SrO:10 17wt%, MoO3+V2O5+WO3Scope:1‑5wt%.The glass has high strain-point(>670℃), low-expansion coefficient (<37×10‑7/ DEG C), high elastic modulus(>80GPa), do not contain alkali-metal feature.
Description
Technical field
The invention belongs to photoelectric display field, relate generally to a kind of ultra-thin glass as TFT-LCD display base plates and its
Preparation method.
Background technology
Terminal of the display as presentation of information, plays a very important role in information-intensive society construction.Enter 21 generation
Since discipline, the advantages of flat panel display and products thereof is with its lightening, high definition, in electronical display product (such as notebook
Computer, LCD TV) etc. aspect obtained fast development, gradually instead of now traditional cathode ray tube (Cathode
Ray Tube, abbreviation CRT) type tv product.
Lcd technology due to its ripe preparation technology, inexpensive and outstanding display performance, in flat pannel display city
Leading position is occupied in.Common liquid crystal display is divided into 4 kinds by physical arrangement:Twisted nematic (TN-Twisted
Nematic);Super-twist nematic (STN-Super TN);Double-layer super-twist nematic (DSTN-Dual Scan
Tortuosity Nomograph);Film transistor type (TFT--Thin Film Transistor).Tft liquid crystal
Display (Thin Film Transistor-Liquid Crystal Display, abbreviation TFT-LCD) is because of its response time
Hurry up, have outstanding color saturation, a reducing power, and its effective display size is big, good environmental protection, small volume, clear
The features such as clear degree is high, becomes the Miniature Terminal such as mobile phone, MP3 player, automatic navigator display device and TV, notebook electricity
Main flow display device on brain, desktop computer, occupies leading position in liquid crystal display.
In LCD Structure of thin film transistor, panel is the core of whole display, and which can be considered two panels
One layer of liquid crystal of glass substrate sandwich, the glass substrate on upper strata are combined with colored filter (Color Filter), lower floor
Glass substrate then have transistor to be embedded in.And base plate glass participates in the processing procedure process of whole TFT-LCD, its performance, matter
Panel quality in amount appreciable impact, and therefore the display effect of display is largely affected by glass substrate.
The TFT-LCD of commercialization at present shows glass substrate Quality and property requirement following points:
(1) belong to the glass composition of alkali metal-free oxide, to avoid due to the alkali gold in glass in heating process
Category ion is diffused in the semi-conducting material of precipitation, is damaged quasiconductor and film performance, is caused short circuit and make micro structure
Thin film transistor (TFT) " is poisoned ".
(2) base plate glass requires thermalexpansioncoefficientα30/380=(32~38) × 10-7/ K, because needing reduction base plate glass to exist
The thermal stress for producing in heating process repeatedly, and need and polysilicon and amorphous si film material thermal expansion coefficient phase
Match somebody with somebody.
(3) base plate glass should have good chemical stability, the cleaning and etching of resistant to many chemical solution.
(4) base plate glass strain point should be not less than 650 DEG C, prevent base plate glass in heat treatment process from shrinking and deforming.
(5) base plate glass density p≤2.6g/cm3, elastic modulus E > 72GPa (7.2kg/mm2), send out in large scale screen
Under the exhibition general trend of events, the advantage of Portable durable is kept.
In the published display glass glass substrate patent at present, glass surface tension is ignored in process of production
Material impact.Such as the glass composition described in 101066836 A of Chinese patent CN with high temperature and chemical stability and its
Exemplifications set out in preparation method, although strain point of glass temperature is higher, glass propertiess are good, but do not account for glass and melt
Material impact of the surface tension of body in Improving Glass Manufacturing Processes, have impact on its commercial application value, for another example United States Patent (USP)
In alkali-free glass substrate described in US20090270242A1, raise containing the recrystallization temperature for promoting glass, increase glass table
The ZrO of face tension force2, it is unfavorable for the operation of glass production, while also causing the glass melting temperature of glass to raise, makes the energy of glass production
Consumption increases.TFT-LCD base plate glass is high to production technology technical requirements as a kind of ultra-thin glass, and the surface of glass melt
Power is the fundamental parameter in Improving Glass Manufacturing Processes.During glass clarifying, micro-bubble in the presence of surface tension,
It is dissolvable in water in vitreous humour, during glass drawing is thin, edge machine will overcome capillary effect, through drawing repeatedly thin ability
Requirement is reached, energy consumption is increased.
The purpose of the present invention is by adding the capillary oxide of multiple reductions, is ensureing not affecting properties
Under the conditions of, reduce glass surface tension, edge machine job stability can be increased, ultra-thin glass percent ripple and thickness is advantageously reduced
Difference, and reduces energy consumption, so as to the low surface of high intensity for preparing a kind of requirement for meeting modern market environmental protection, being suitable for display
The glass substrate of tension force.
Content of the invention
It is an object of the invention to provide a kind of high intensity for being suitable for display, the ultra-thin glass of low surface tension and its system
Preparation Method, the glass have high strain-point (>670 DEG C), low-expansion coefficient (<37×10-7/ DEG C), high elastic modulus (>80GPa)、
Alkali-metal feature is not contained.
For achieving the above object, the technical solution used in the present invention is:A kind of ultra-thin glass of low surface tension (or claim
For:A kind of ultra-thin glass as TFT-LCD substrates), it is characterised in that its chemical composition (wt.%) by weight percentage is:
Wherein SiO2+Al2O3Scope:The scope of 77-85wt.%, MgO+CaO+SrO:10-17wt%, MoO3+V2O5+
WO3Scope:1-5wt%.
In the present invention, SiO2It is the main body of glass formation skeleton, is the composition played a major role in glass skeleton.SiO2's
Mass percent (wt.%) is 58-68, SiO2Content is difficult to obtain low bulk, the glass of high strain-point, meeting less than 58wt.%
Reduce the chemical-resistant stability of glass;SiO2When content is higher than 68wt.%, the high-temperature viscosity of glass can increase, and cause glass
Glass melting temperature is too high.
Al2O3Belong to the intermediate oxide of glass, Al3+There are two kinds of co-ordination states, that is, be located in tetrahedron or octahedron,
When oxygen is enough in glass, aluminum-oxygen tetrahedron [AlO is formed4], continuous network is formed with silicon-oxy tetrahedron, when oxygen in glass
When not enough, alumina octahedral [AlO is formed6], it is in the hole that network outer body is in silica structure network, so necessarily containing
In the range of amount can and SiO2It is the main body of glass network formation.Al2O3Mass percent (wt.%) be 16-24.Al2O3Contain
Amount is difficult to obtain high strain-point, high strength glass less than 16wt.%, and the chemical-resistant stability of glass is not enough, while glass can be increased
The crystallization tendency of glass;Al2O3Content can dramatically increase glass high-temperature viscosity more than 24wt.%, raise the glass melting temperature of glass.
B2O3And network former, and the composition of composition glass skeleton, while be a kind of reduction glass smelting again
The cosolvent of viscosity.Boron oxygen triangle body [BO3] and boron oxygen tetrahedron [BO4] it is structural component, boron may be with three at different conditions
Angle body [BO3] or boron oxygen tetrahedron [BO4] exist, in high temperature melting condition, it is generally more difficult to form boron oxygen tetrahedron, and can only
Deposited in the way of trihedral, but in low temperature, under certain condition B3+Have and capture free oxygen and form tetrahedral trend, make structure
Closely improve the low temperature viscosity of glass, but have high temperature to reduce the characteristic that glass viscosity and low temperature improve glass viscosity due to it,
Also determine that its content range is less.B2O3Percentage by weight (wt.%) be 5-12.B2O3Content be less than 5wt.%, nothing
Method plays a part of hydrotropy, while increasing the thermal coefficient of expansion of glass, reduces the chemical stability of glass;B2O3Content be more than
12wt.%, can reduce the strain point of glass, while making the split-phase of glass be inclined to increase.
MgO is glass structure network modifying oxide, reduces thermal coefficient of expansion, and the percentage by weight (wt.%) of MgO is 2-
7, MgO content can increase the tendency towards devitrification of glass when being more than 7wt.%, acid resistance reduces.
CaO is glass structure network modifying oxide, and the percentage by weight (wt.%) of CaO is 2-9, and the content of CaO is more than
9wt.%, can reduce glass chemical-resistant stability, increase the thermal coefficient of expansion of glass.
SrO is glass structure network modifying oxide, plays a part of to suppress glass phase-separating, strengthens acid resistance, the weight of SrO
Amount percentage ratio (wt.%) is 3-13, can increase chemical durability of glass and improve glass when the content of SrO is more than 13wt.%
Thermal coefficient of expansion.
MoO3It is glass structure network modifying oxide, MoO3Percentage by weight (wt.%) be 1-4, glass can be reduced
Transition point and surface tension, but work as MoO3During more than 4wt.%, split-phase is also easy to produce, increases devitrification of glass tendency, MoO3It is less than
During 1wt.%, the effect for significantly reducing glass surface tension is not had.
V2O5It is glass structure Network former oxide, V2O5Percentage by weight (wt.%) be 0-2, can be with petition of surrender face
Tension force, but work as V2O5During more than 2wt.%, devitrification of glass is easily caused, glass coloration is made.
WO3It is glass structure network intermediate oxide, thermal expansion coefficient of glass can be reduced, drops surface tension, WO3Weight
Amount percentage ratio (wt.%) is 0-3, but works as WO3During more than 3%, glass density can be increased
SiO in the present invention2+Al2O3Optimum range:77-85wt.%, is then unfavorable for obtaining low bulk, height less than 77wt.%
Strain-point glass, the glass of high elastic modulus, the chemical-resistant stability of glass is not enough, and more than 85wt.%, then temperature founded by glass
Height is spent, liquidus temperature increases, and does not utilize molding.
MgO+CaO+SrO optimum ranges:10-17wt%, when content is more than 17wt.%, can cause thermal coefficient of expansion to increase,
And cause glass density to increase, when content is less than 10wt.%, do not have the effect that fluxes.
MoO3+V2O5+WO3Optimum range:1-5wt%, when content is more than 5wt.%, can cause glass coloration, when content low
In 1wt.%, not having reduces the effect of glass surface tension.
The preparation method of the ultra-thin glass of above-mentioned a kind of low surface tension, it is characterised in that comprise the steps:
1) by chemical composition and percentage by weight (wt.%) it is:
Wherein SiO2+Al2O3Scope:The scope of 77-85wt.%, MgO+CaO+SrO:10-17wt%, MoO3+V2O5+
WO3Scope:1-5wt%;Choose raw material (making which meet chemical composition);
2) pour the raw material of selection into platinum crucible, melt 12~24 hours at a temperature of 1630 DEG C, clarifier is oxidation
Stannum, obtains melten glass liquid;
3) melten glass liquid is cast, is then annealed, then be ground and polish, obtain the ultra-thin of low surface tension
Glass.
Described ultra-thin glass belongs to high-aluminum alkali-free glass.Described ultra-thin glass thickness can be less than or equal to 0.7 millimeter.
The swollen swollen factor alpha of described ultra-thin glass30/380In (32~37) × 10-7In the range of/K.The glass chemistry component is dirty to environment
Dye is little.
Ultra-thin in the present invention, it is adaptable to the technique productions such as float glass process, press over system and slot draw method, and there is following thing
Physicochemical performance:Thermal coefficient of expansion is less than 37 × 10-7/ DEG C (30~380 DEG C), density are less than 2.5g/cm3, strain point is more than 670
DEG C, Young's modulus of elasticity is higher than 80GPa, is 320mN/m in 1200 DEG C of average surface tensions, than general commercialization ultra-thin glass table
The low 40mN/m of face tension force.
The ultra-thin glass of low surface tension according to the present invention is suitable for float process technique, and due to its surface tension
Low, edge machine job stability can be increased, ultra-thin glass percent ripple is advantageously reduced and thickness is poor.
The invention has the beneficial effects as follows:Compared with the alkali-free liquid crystal substrate glass of prior art, first, glass melt surface
Tension force is low, can increase edge machine job stability, advantageously reduces ultra-thin glass percent ripple and thickness is poor;Average at 1200 DEG C
Surface tension is 320mN/m, 40mN/m lower than general commercialization ultra-thin glass surface tension force;Second, thermal coefficient of expansion is low, strain point
Height, can effectively prevent base plate glass bursting, shrinking, deforming and warpage in process of production;3rd, glass density is low, can
Effectively to mitigate the weight of display, it is easy to keep the large-scale development;4th, Young's modulus of elasticity is higher than 80GPa, mechanical strength
Height, is conducive to slimming development;5th, chemical stability is good, advantageously ensures that etching quality;6th, glass chemistry is constituted
In do not contain heavy metal BaO, As2O3, the harmful substance such as halogen Cl, impact will not be produced on environment and health of human body.
Specific embodiment
Embodiment 1
First, by 1 embodiment of table, 1 glass composition selection raw material, ingredient requirement, (150 μm of oversizes are 1wt% to quartz sand
Below, 45 μm of siftage are below 30wt%, Fe2O3Content be less than 0.01wt%), aluminium oxide (50 μm of mean diameter), boric acid or
Boric anhydride (it is below 10wt% that 400 μm of oversizes are below 10wt%, 200 μm of siftage), Calcium Carbonate (250 μm of mean diameter),
Strontium nitrate or strontium carbonate (50 μm of mean diameter), magnesium oxide (60 μm of oversizes of mean diameter are below 1wt%), molybdenum trioxide
(45 μm of oversizes of mean diameter are below 1wt%), the alkali metal oxide content in raw material are less than 0.1wt%, five oxidations two
Vanadium (50 μm of mean diameter), Tungstic anhydride. (50 μm of mean diameter).And Fe in frit2O3Strictly controlled, finished product glass
Glass Fe2O3Content is less than 150ppm.Clarifier is stannum oxide so as to which dispensing meets the glass chemistry composition of table 1, then using platinum
Golden crucible is melted 12~24 hours at a temperature of 1630 DEG C.After melting, melten glass liquid is cast into the test article of regulation
Require, then annealed.It is ground again and polishes, makes glass specimen.As shown in table 1, (1) density is its test performance
2.44g/cm3;(2) 30-380 DEG C of average coefficient of linear expansion 34.2 × 10-7/℃;(3) strain point Tst is 700 DEG C;(4) anneal
Point Ta is 765 DEG C;(5) liquidus temperature TLFor 1113 DEG C;(6) elastic modelling quantity is 84.2GPa;(7) hydrofluoric acid resistant buffer is rotten
Corrosion 0.28mg/cm2;(8) glass 1200 DEG C surface tension be 322mN/m.
Wherein, the density p of glass is determined using Archimedes method;30-380 DEG C of linear expansion coefficient adopts horizontal expander instrument
Measurement, is represented with average coefficient of linear expansion, the measuring method specified using ISO 7991;The strain point of glass adopts ASTM
The camber beam method measurement of C598 defineds;The elastic modelling quantity of glass is measured using the method for ASTM C623 defineds;The surface of glass
Tension force foundation Young-Laplace formula, by testing high temperature molten glass contact angle, through DSA analysis software Accurate Curve-fittings
Calculating is tried to achieve.
Embodiment 2
The actual composition of glass, using raw material same as Example 1 and ingredient requirement and is taken with reference to 1 embodiment 2 of table
Identical melting process system and test condition, in the key property that table 1 shows sample.(1) density is 2.47g/cm3;(2)
30-380 DEG C of average coefficient of linear expansion 33.8 × 10-7/℃;(3) strain point Tst is 684 DEG C;(4) annealing point Ta is 757 DEG C;
(5) liquidus temperature TLFor 1121 DEG C;(6) elastic modelling quantity is 84.5GPa;(7) hydrofluoric acid resistant buffer corrosivity 0.32mg/
cm2;(8) glass 1200 DEG C surface tension be 324mN/m.
Embodiment 3
The actual composition of glass, using raw material same as Example 1 and ingredient requirement and is taken with reference to 1 embodiment 3 of table
Identical melting process system and test condition, in the key property that table 1 shows sample.(1) density is 2.5g/cm3;(2)30-
380 DEG C of average coefficient of linear expansion 35.2 × 10-7/℃;(3) strain point Tst is 695 DEG C;(4) annealing point Ta is 759 DEG C;(5)
Liquidus temperature TLFor 1116 DEG C;(6) elastic modelling quantity is 84.3GPa;(7) hydrofluoric acid resistant buffer corrosivity 0.30mg/cm2;
(8) glass 1200 DEG C surface tension be 324mN/m.
Embodiment 4
The actual composition of glass, using raw material same as Example 1 and ingredient requirement and is taken with reference to 1 embodiment 4 of table
Identical melting process system and test condition, in the key property that table 1 shows sample.(1) density is 2.49g/cm3;(2)
30-380 DEG C of average coefficient of linear expansion 35.9 × 10-7/℃;(3) strain point Tst is 702 DEG C;(4) annealing point Ta is 766 DEG C;
(5) liquidus temperature TLFor 1123 DEG C;(6) elastic modelling quantity is 83.6GPa;(7) hydrofluoric acid resistant buffer corrosivity 0.28mg/
cm2;(8) glass 1200 DEG C surface tension be 318mN/m.
Embodiment 5
The actual composition of glass, using raw material same as Example 1 and ingredient requirement and is taken with reference to 1 embodiment 5 of table
Identical melting process system and test condition, in the key property that table 1 shows sample.(1) density is 2.44g/cm3;(2)
30-380 DEG C of average coefficient of linear expansion 36.2 × 10-7/℃;(3) strain point Tst is 679 DEG C;(4) annealing point Ta is 753 DEG C;
(5) liquidus temperature TLFor 1109 DEG C;(6) elastic modelling quantity is 85.1GPa;(7) hydrofluoric acid resistant buffer corrosivity 0.40mg/
cm2;(8) glass 1200 DEG C surface tension be 316mN/m.
Especially, it should be noted that, certain can be not limited solely in any combination between various embodiments of the present invention
Specific combination.In the following table, comparative example 1 is that a glass ingredient in Chinese patent CN 102030475A, comparative example 2 are
The AN100 trade mark glass of Japanese Asahi companies manufacture, comparative example 3 is 1737 boards manufactured by Corning Incorporated
Flint glass F, and the method with reference to surface tension, elastic modelling quantity, resistance to compression/rupture strength test in embodiment 1, to these three groups
Glass is divided to be tested, test result is as shown in table 1.
Table 1
Table 1 is illustrated:Glass surface tension of the present invention is low, and the glass have high strain-point (>670 DEG C), low bulk system
Number (<37×10-7/ DEG C), high elastic modulus (>80GPa), alkali-metal feature is not contained.
It should be appreciated that the various embodiments of glass of the present invention composition go for its present invention application,
Base plate glass and the preparation method of base plate glass, it is possible to the various combination of embodiment with them.
The bound of the glass composition cited by the present invention, interval value can realize the present invention, numerous to list herein
Embodiment.
Claims (2)
1. a kind of ultra-thin glass of low surface tension, it is characterised in that its chemical composition is by weight percentage:
Wherein SiO2+Al2O3Scope:The scope of 77-85wt.%, MgO+CaO+SrO:10-17wt%, MoO3+V2O5+WO3's
Scope:1-5wt%.
2. a kind of preparation method of the ultra-thin glass of low surface tension as claimed in claim 1, it is characterised in that including as follows
Step:
1) by chemical composition and percentage by weight it is:
Wherein SiO2+Al2O3Scope:The scope of 77-85wt.%, MgO+CaO+SrO:10-17wt%, MoO3+V2O5+WO3's
Scope:1-5wt%;Choose raw material;
2) pour the raw material of selection into platinum crucible, melt 12~24 hours at a temperature of 1630 DEG C, clarifier is stannum oxide, obtains
Arrive melten glass liquid;
3) melten glass liquid is cast, is then annealed, then be ground and polish, obtain the ultra-thin glass of low surface tension
Glass.
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