CN104326662B - A kind of alkali-free alumina silicate glass of not boracic - Google Patents
A kind of alkali-free alumina silicate glass of not boracic Download PDFInfo
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- CN104326662B CN104326662B CN201310749563.6A CN201310749563A CN104326662B CN 104326662 B CN104326662 B CN 104326662B CN 201310749563 A CN201310749563 A CN 201310749563A CN 104326662 B CN104326662 B CN 104326662B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
- C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
- C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
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Abstract
A kind of alkali-free alumina silicate glass of not boracic, solve boron oxide in existing alkali-free alumina silicate glass and cause that strain point of glass reduction, glass density be big, elastic modelling quantity is not high enough and fining agent improper use technical problem, the technical scheme of use is, the constituent of the alkali-free glass and includes by mole proportioning is calculated：SiO268.5 ~ 72.5 %, Al2O312.5 ~ 16%, MgO 2 ~ 6 %, CaO 3.5 ~ 5.5%, SrO 0.5 ~ 3.5%, BaO 1 ~ 5%, ZnO 0.5 4%.The present invention has chemical stability higher, with strain point higher, with Young's modulus higher, with ratio modulus higher, with transmitance higher, with relatively low fusion temperature, with relatively low liquidus temperature, with relatively low density.
Description
Technical field
The invention belongs to glass manufacturing area, it is related to a kind of alkaline earth aluminates glass and its component, not alkali metal containing.This
Invention is a kind of environmental type glass, with chemical stability and mechanical performance higher；With the relatively low coefficient of expansion and
Liquidus temperature；It is widely portable to make glass substrate, photovoltaic device or other phototubes that plane shows and illuminates
The industry glass composition such as the glass substrate of part, glass.Particularly a kind of alkali-free alumina silicate glass of not boracic.
Background technology
With the fast development of photovoltaic industry, the demand to various display devices constantly increases, such as active matrix
The active matrix liquid crystal display device of liquid crystal display, Organic Light Emitting Diode and application low-temperature polysilicon silicon technology, these displays
Device is all based on using thin film semiconductor material to produce thin-film transistor technologies.The silicon substrate TFT of main flow can be divided into non-crystalline silicon tft,
Multi-crystal TFT and monocrystalline silicon TFT, wherein non-crystalline silicon tft are the technology of present main flow TFT-LCD applications, non-crystalline silicon tft technology
Treatment temperature in procedure for producing can be completed at a temperature of 300 ~ 450 DEG C.And LTPS multi-crystal TFTs are needed in the fabrication process
Repeatedly to process at relatively high temperatures, substrate must can not deform in multiple high temp processing procedure, and this is just to substrate glass
Glass performance proposes requirement higher, and preferred strain point is higher than 650 DEG C, more preferably above 670 DEG C, 700 DEG C, 720 DEG C,
So that substrate in panel processing procedure have as far as possible small thermal contraction, therefore the strain point temperature of substrate the higher the better.While glass
The thermal coefficient of expansion of substrate needs the similar thermal expansion coefficient with silicon, and stress and destruction are reduced as far as possible, therefore base plate glass is excellent
The thermal linear expansion coefficient of choosing is 28 ~ 39 × 10-7/ DEG C between.For the ease of production, production cost is reduced, as display base
The glass of plate should have relatively low fusion temperature and liquidus temperature.
The glass substrate shown for plane is, it is necessary to pass through the technologies such as sputtering, chemical vapor deposition in underlying substrate glass
Surface forms nesa coating, dielectric film, semiconductor film and metal film, then forms various circuits and figure by optical lithography
Shape, if glass contains alkali metal oxide, alkali metal ion diffuses into deposited semiconductor material, meeting in heat treatment process
Infringement semiconductor film characteristic, therefore, TFT glass should be free of alkali metal oxide.Prior art, it is preferred that with SiO2、
Al2O3、B2O3, alkaline earth oxide MgO, CaO, SrO etc. be the alkaline earth aluminates glass of principal component.
The strain point of most of silicate glasses is with the increase of glass former content and the reduction of modifier content
Increase.But can cause high temperature melting and clarification difficult simultaneously, cause refractory corrosion to aggravate, increase energy consumption and production cost.
Therefore, improved by component so that low temperature viscosity will also ensure that high temperature viscosity is not in big lifting while increase, or even
Reduction is only the optimal breach for improving strain point.
In high-aluminum alkali-free silicate glass system, boron oxide B is added2O3Good fluxing effect can be brought, while having
Beneficial to lifting glass endurance.But in low temperature viscosity area, B2O3But so that strain point of glass is significantly reduced, then how simultaneously
Improving the endurance and strain point temperature of glass substrate just turns into a difficult problem of long-standing problem those skilled in the art.
In the process of glass substrate, base plate glass is horizontal positioned, and glass has certain journey under Gravitative Loads
That spends is sagging, and sagging degree is directly proportional to the density of glass and the elastic modelling quantity of glass is inversely proportional.With substrate manufacture towards
Large scale, the development in slimming direction, the sagging of glass plate must draw attention in manufacture.Therefore composition should be designed, makes substrate
Glass has alap density and elastic modelling quantity as high as possible.
With the popularization of smart mobile phone and panel computer, the epoch of intelligent mobile are opened.Conventional mobile phone is confined to lead to
Communication function, but it is close with notebook with the performance of the smart machine of panel computer including smart mobile phone at present, and people rely on nothing
The convenience of line communication, is not performing and is enjoying the commercial affairs and recreation of higher level all the time.Under such trend,
Requirement to display performance is also being improved constantly, image quality especially to intelligent movable equipment, visuality out of doors
Can require also lifted, while the use burden in order to mitigate portable equipment, weight, thickness are thinning as can not keep away
The main trend exempted from.Under the guiding of this trend, the direction that display panel is showing to lightening, ultra high-definition is developed, face
Plate making technology manages temperature development to higher height；Simultaneously monolithic glass by PROCESS FOR TREATMENT, thickness reach 0.25mm, 0.2mm,
0.1mm is even more thin.Make the thinning mode of glass presently mainly chemical reduction, specifically, use hydrofluoric acid or hydrofluoric acid
Buffer solution corrodes to glass substrate, and its thinning principle is as follows：
Main chemical reactions：4HF+SiO2=SiF4+2H2O,
Secondary chemical reaction：RO+2H+=R2++H2O（R represents alkaline-earth metal etc.）.
Surface quality after chemical reduction technique and thinning glass substrate has certain relation with parent glass composition, existing
TFT-LCD base plate glass frequently occurs the bad deficient point such as " pit ", " sags and crests ", it is necessary to carry out secondary during chemical reduction
Polishing is directly discarded, and increased the production cost of glass substrate.Glass with chemical stability high tool after thinning
There is more preferable surface quality, therefore research and develop the TFT-LCD base plate glass of high chemical stability, it is possible to reduce second polishing etc. is produced
Cost, lifts product quality and yields, has larger benefit for large industrialized production.
With the development of lightening trend, in the more advanced lines glass substrate productions such as G5 generations, G6 generations, G7 generations, G8 generations, water
The glass substrate of placing flat due to deadweight produce it is sagging, be warped into emphasis research topic.For the glass substrate producer,
Will be by various links such as annealing, cutting, processing, inspection, cleanings after glass board material shaping, the sagging of sized rectangular glass substrate will
Influence the ability for loading, taking out and separating in the casing for transported between processing stand glass.It is similar for counter plate manufacturer
Problem is equally existed.Larger sag or warpage can cause fragment rate to improve and the alarm of CF making technologies, have a strong impact on product
Yield.If at two ends supporting substrate both sides, the maximum sag of chain of glass substrate（S）Can be expressed as follows：
K is constant, and ρ is density, and E is elastic modelling quantity, and l is spaced for support, and t is thickness of glass substrate.Wherein, (ρ/E) is
Than the inverse of modulus.Than the ratio that modulus refers to elasticity modulus of materials and density, also known as " than elastic modelling quantity " or " specific stiffness ",
It is structure design to one of important requirement of material.Material weight is lighter under explanation same stiffness higher than modulus, or phase homogeneity
The lower rigidity of amount is bigger.From above formula, when the timing of l, t mono-, ρ diminishes after E is increased can reduce sag of chain, therefore should make substrate
The as far as possible low density of glass tool and elastic modelling quantity as far as possible high, i.e., with as far as possible big ratio modulus.Glass after thinning is due to thickness
That spends strongly reducing and mechanical strength reduction occurs, it is easier to deform.Density, increase are reduced than modulus and intensity, glass is reduced
Fragility turns into the factor that glass production person needs emphasis to consider.
Use on fining agent：In order to obtain still alkali-free glass, using fining gases, expelled from glass melts
The gas produced during glass reaction, increases alveolar layer, it is necessary to reuse the fining gases of generation when fusing is homogenized in addition
Footpath, makes it float, and thus takes out the small bubble of participation.
But, the viscosity of the glass melts as glass substrate for plane display device is high, need to be with higher temperature melting.
In this kind of glass substrate, generally cause Vitrification at 1300 ~ 1500 DEG C, more than 1500 DEG C at a high temperature of deaeration,
Matter.Therefore, in fining agent, widely using can produce clarification gas between temperature range wider, i.e., 1300 ~ 1700 DEG C
The As of body2O3.But, As2O3Toxicity it is very strong, glass manufacturing process or cullet treatment when, it is possible to pollute ring
Border and the problem of health is brought, it is using being restricted.In the prior art, once trial is clarified with antimony clarification come substitute for arsenic.
However, antimony there is also in itself influence environment and health in terms of problem.Although Sb2O3Toxicity unlike As2O3It is high like that, but
Sb2O3It is still virose.And compared with arsenic, antimony produces the temperature of fining gases relatively low, removes having for this kind of glass blister
Effect property is relatively low.
Therefore, how to obtain it is a kind of with endurance higher, high strain-point, low-density, high elastic modulus base plate glass
As a great problem for being stranded right those skilled in the art.
The content of the invention
The present invention is that boron oxide causes strain point of glass reduction, glass density in solving existing alkali-free alumina silicate glass
Greatly, elastic modelling quantity is not high enough and technical problem of fining agent improper use, there is provided a kind of environmentally friendly, performance is more perfect
Not boracic alkali-free alumina silicate glass, in the glass ingredient, even if without B2O3, glass substrate is still with compared with Gao Naihua
Property, even if fining agent does not use As2O3And Sb2O3, also in the absence of the formula of the glass substrate as surface defect.Matched somebody with somebody using this
The obtained glass substrate in side meets environmental requirement, without As2O3、Sb2O3And its compound, while the glass has change higher
Stability is learned, with strain point higher, with Young's modulus higher, with ratio modulus higher, with transmission higher
Rate, with relatively low fusion temperature, with relatively low liquidus temperature, with relatively low density, meets FPD industry hair
Exhibition trend, is suitable for various molding modes such as fusion glass tube down-drawing, float glass process and manufactures.
The present invention is to realize that the technical scheme that goal of the invention is used is, a kind of alkali-free alumina silicate glass of not boracic, its
It is critical only that：The constituent of the alkali-free glass and by mole calculate proportioning include：
SiO268.5 ~ 72.5 %,
Al2O312.5 ~ 16%,
The % of MgO 2 ~ 6,
CaO 3.5 ~ 5.5%,
SrO 0.5 ~ 3.5%,
BaO 1 ~ 5%,
ZnO 0.5-4%。
The beneficial effects of the invention are as follows：1st, the present invention has environment friendly, without any poisonous and harmful substance, fining agent
Using stannous oxide SnO, SnO is readily available material, and known without detrimental nature, and it is used alone as glass fining agent
When, there is the temperature range of generation fining gases higher, it is adapted to the elimination of this kind of glass blister；2nd, by controlling SiO2+Al2O3>
83%、MgO/R’O<0.4、ZnO/R’O<0.4、(MgO+ZnO)/R’O>0.3、0.8<Al2O3/R’O<1.0, glass can be made to have simultaneously
There are chemical stability higher, strain point, Young's modulus, spy more excellent than modulus and relatively low fusion temperature, liquidus temperature etc.
Property；3rd, the glass substrate of the glass ingredient formula production provided by means of the present invention, can reach following technology and refer to after testing
Mark：10%HF acid solutions（22℃/20min）Erosion amount<4.5mg/cm2；50~350 degree of thermal coefficient of expansions be 31~38 ×
10-7/℃；Strain point is more than 740 DEG C；Density is less than 2.65g/cm3, liquidus temperature be less than 1140 DEG C, per kilogram glass base
Bubbles number of the bubble diameter in ＞ 0.1mm is invisible in plate；4th, due to the SiO higher contained in instant component2With Al2O3
B is free of in resultant, and component2O3, it is ensured that high strain-point, a certain proportion of MgO+ZnO that arranges in pairs or groups can effectively reduce fusing temperature
Degree, brings larger space, while the production cost such as fuel, electric power is also minimized to producing line Yield lmproved.
Specific embodiment
A kind of alkali-free alumina silicate glass of not boracic, it is critical only that：The constituent of the alkali-free glass and massage
Your percentage calculates proportioning to be included：
SiO268.5 ~ 72.5 %,
Al2O312.5 ~ 16%,
The % of MgO 2 ~ 6,
CaO 3.5 ~ 5.5%,
SrO 0.5 ~ 3.5%,
BaO 1 ~ 5%,
ZnO 0.5-4%。
By mole calculating in the constituent of the alkali-free glass：SiO2+Al2O3>83%。
By mole calculating in the constituent of the alkali-free glass： MgO/R’O<0.4, wherein, R ' O=MgO+
CaO+SrO+BaO+ZnO。
By mole calculating in the constituent of the alkali-free glass：ZnO/R’O<0.4, wherein, R ' O=MgO+CaO
+SrO+BaO+ZnO。
By mole calculating in the constituent of the alkali-free glass：(MgO+ZnO)/R’O>0.3, wherein, R ' O=
MgO+CaO+SrO+BaO+ZnO。
By mole calculating in the constituent of the alkali-free glass：0.8< Al2O3/R’O <1.0, wherein, R ' O=
MgO+CaO+SrO+BaO+ZnO。
Also contain SnO in the constituent of the alkali-free glass, with Mole percent gauge, the addition scope of SnO is：0.05
~0.1%。
By mole calculating in the constituent of the alkali-free glass：Al2O3Preferred scope be 13 ~ 14.5%.
By mole calculating in the constituent of the alkali-free glass：The preferred scope of ZnO is 0.6 ~ 3%.
By mole calculating in the constituent of the alkali-free glass：SiO2Preferred scope be 69 ~ 71%.
The present invention will first include the raw material of above-mentioned each glass substrate correspondence oxide molar percent composition when implementing
After uniform stirring mixing, then by mixed material melt-processed, stir discharge bubble with platinum rod and be homogenized glass metal, then will
Its temperature is reduced to the glass substrate forming temperature range required for being molded, and by annealing theory, producing flat-panel screens needs
The thickness of the glass substrate wanted, then to be molded glass substrate carry out simple cold work, finally to the base of glass substrate
This physical characteristic carries out test turns into qualified products.
In the present invention, SiO2Molar content be 68.5~72.5%.SiO2It is glass former, if content is too low, no
Beneficial to the corrosive enhancing of endurance, the coefficient of expansion can be made too high, the easy devitrification of glass；Improve SiO2Content contributes to glass light
Quantify, thermal coefficient of expansion reduces, strain point increases, and chemical resistance increases, but high temperature viscosity is raised, and is so unfavorable for melting, one
As kiln be difficult to meet, so SiO2Content be 68.5~72.5%.
Al2O3Molar content be 12.5~16%, be used to improve the intensity of glass structure, if content be less than 12.5%, glass
Easy devitrification, is also easily corroded by extraneous aqueous vapor and chemical reagent.The A1 of high content2O3Contribute to strain point of glass, bending resistance
Intensity increases, but crystallization easily occurs in too high glass, while can cause that glass is difficult to melt, therefore A12O3Content be
12.5~16%.
MgO makes glass be easy to the spy of fusing with glass Young's modulus is substantially improved and than modulus, high temperature viscosity is reduced
Point.When alkaline-earth metal resultant is less in alkali-free silicate glass, the larger network-modifying ion Mg of electric-field intensity is introduced2+, hold
Local accumulation effect is easily produced in the structure, increases nearest neighbour distance.More intermediate oxygen is introduced in this case
Compound Al2O3, with [AlO4] in the presence of state, because these polyhedrons carry negative electricity, attract subnetwork outer cationic, make
The accumulation degree of glass, crystallization ability decline；When alkaline-earth metal resultant is more, network fracture is than in the case of more serious, introducing
MgO, can make the silicon-oxy tetrahedron of fracture reconnect and decline devitrification of glass ability.Therefore add MgO when it is noted that with
The mixing ratio of other components.Relative to other alkaline earth oxides, the presence of MgO can bring the relatively low coefficient of expansion and close
Degree, chemically-resistant higher, strain point and elastic modelling quantity.If MgO is more than 6mol%, glass endurance can be deteriorated, while glass holds
Easy devitrification.Too low content of MgO contrast modulus improves unfavorable.Therefore its content is 2 ~ 6mol%.
The molar content of CaO is 3.5~5.5%, and calcium oxide is used to promote the melting of glass and adjustment glass mouldability.Such as
Fruit calcium oxide content is less than 3.5%, is difficult to reduce the viscosity of glass, and content is excessive, and glass would tend to occur crystallization, thermal expansion system
Number also can greatly amplitude variation greatly, it is unfavorable to successive process.So the content of CaO is 3.5~5.5%.
The molar content of SrO is 0.5~3.5%, and strontium oxide strontia is as flux and prevents glass from crystallization occur, if content
Excessively, glass density can be too high, causes the mole overweight of product.So the content of SrO is defined as 0.5~3.5%.
The content of BaO is 1~5%, and barium monoxide is similar to the effect of strontium oxide strontia, and content is excessive, and the density of glass can become big,
And strain point can be greatly lowered.So the content of SrO is defined as 1~5%.
The molar content of ZnO be 0.5 ~ 4%, bivalent metal oxide according to it in the periodic table of elements status with to property
Influence is different, can be divided into two classes：One class is the alkaline earth oxide for being located at main group, its ion R2+With 8 exoelectron knots
Structure；Equations of The Second Kind is located at periodic table subgroup（Such as ZnO, CdO）, its ion R2+With 18 outer electronic structures, in glass two
The configuration state of person from glass property influence be different.ZnO can reduce glass high temperature viscosity（Such as 1500 degree）, be conducive to
Eliminate bubble；The chemical resistance for have lifting intensity, hardness below softening point simultaneously, increasing glass, reduces glass thermal expansion system
Several effects.In alkali-free glass system, adding appropriate ZnO helps to suppress crystallization, can reduce recrystallization temperature.In theory
On, ZnO is general with [ZnO under high temperature after introducing glass as network outer body in alkali-free glass4] form exist, compared with
[ZnO6] glass structure is more loose, is under the identical condition of high temperature with the glass without ZnO and compared, the glass containing ZnO glues
Degree is smaller, and atomic motion speed is bigger, it is impossible to forms nucleus, it is necessary to further reduce temperature, is just conducive to the formation of nucleus, because
And, reduce the crystallization ceiling temperature of glass.ZnO content excessively can be greatly lowered the strain point of glass.So ZnO's contains
Amount is defined as 0.5 ~ 4 mole of %.
In the present invention, the stannous oxide SnO of 0.05~0.1mol% can also be added with glass composition, it is molten as glass
Fining agent or defrother during solution, to improve the melting mole of glass.If content is excessive, glass substrate devitrification, institute can be caused
0.1mol% is no more than with its addition.
The specific embodiment that each component is measured with molar percentage in being formulated is given below：
Table 1：
Claims (8)
1. a kind of alkali-free alumina silicate glass of not boracic, it is characterised in that：The constituent of the alkali-free glass and by mole
Percentage calculates proportioning：
SiO268.5 ~ 72.5 %,
Al2O312.5 ~ 13.3%,
The % of MgO 3.6 ~ 6,
CaO 3.5 ~ 5.5%,
SrO 0.5 ~ 3.5%,
BaO 3.7 ~ 5%,
ZnO 0.5-4%；
By mole calculating in the constituent of the alkali-free glass：SiO2+Al2O3>83%；
By mole calculating in the constituent of the alkali-free glass：MgO/R’O<0.4, wherein, R ' O=MgO+CaO+SrO
+BaO+ZnO。
2. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in by mole calculating：ZnO/R’O<0.4, wherein, R ' O=MgO+CaO+SrO+BaO+ZnO.
3. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in by mole calculating：(MgO+ZnO)/R’O>0.3, wherein, R ' O=MgO+CaO+SrO+BaO+ZnO.
4. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in by mole calculating：0.8< Al2O3/R’O <1.0, wherein, R ' O=MgO+CaO+SrO+BaO+ZnO.
5. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in also contain SnO, with Mole percent gauge, the addition scope of SnO is：0.05~0.1%.
6. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in by mole calculating：Al2O3Preferred scope be 13 ~ 13.3%.
7. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in by mole calculating：The preferred scope of ZnO is 0.6 ~ 3%.
8. the alkali-free alumina silicate glass of a kind of not boracic according to claim 1, it is characterised in that：The alkali-free glass
Constituent in by mole calculating：SiO2Preferred scope be 69 ~ 71%.
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| CN105502928B (en) * | 2015-12-30 | 2018-12-11 | 东旭科技集团有限公司 | A kind of alumina silicate glass composition and application thereof |
| CN107129142B (en) * | 2017-04-18 | 2021-02-09 | 东旭光电科技股份有限公司 | Alkali-free glass substrate and preparation method thereof |
| CN107032604A (en) * | 2017-04-18 | 2017-08-11 | 东旭科技集团有限公司 | Glass composition, alkaline earth aluminates glass and its preparation method and application |
| EP3810558B1 (en) * | 2018-06-19 | 2023-04-26 | Corning Incorporated | High strain point and high young's modulus glasses |
| CN114174234A (en) * | 2019-06-26 | 2022-03-11 | 康宁公司 | Alkali-free glass insensitive to thermal history |
| CN112174521A (en) * | 2020-10-30 | 2021-01-05 | 中南大学 | Alkali-free boroaluminosilicate glass for TFT-LCD substrate and preparation method thereof |
| CN112811811A (en) * | 2021-03-07 | 2021-05-18 | 宜山光电科技(苏州)有限公司 | For making polarization3Glass of He gas container and manufacturing method thereof |
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| CN102066273A (en) * | 2008-05-13 | 2011-05-18 | 康宁股份有限公司 | Rare-earth-containing glass material and substrate and device comprising such substrate |
| CN103347832A (en) * | 2011-02-08 | 2013-10-09 | 旭硝子株式会社 | Glass composition, glass substrate for solar cells using glass composition, and glass substrate for display panel |
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