CN108947237A - A kind of alkali-free silicate glass of low-expansion coefficient high strain-point - Google Patents

A kind of alkali-free silicate glass of low-expansion coefficient high strain-point Download PDF

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Publication number
CN108947237A
CN108947237A CN201810844721.9A CN201810844721A CN108947237A CN 108947237 A CN108947237 A CN 108947237A CN 201810844721 A CN201810844721 A CN 201810844721A CN 108947237 A CN108947237 A CN 108947237A
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glass
alkali
expansion coefficient
silicate glass
low
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兰静
王答成
曾召
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Irico Display Devices Co Ltd
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Irico Display Devices Co Ltd
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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
    • 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
    • C03C4/00—Compositions for glass with special properties

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a kind of alkali-free silicate glasses of low-expansion coefficient high strain-point.The glass defines the chemical constituent of each oxide, wherein by main component SiO2It limits in a certain range, while improving strain point of glass, ensure that the chemical stabilities such as the acid resistance of glass；Define SiO2With Al2O3Mass percent summation can be improved the strain point and elasticity modulus of glass, increase the chemical stability of glass.It is substantially free of alkali metal oxide in the glass ingredient, ensure that the stability of thin film transistor (TFT) grid voltage；Glass density in the chemical constituent is lower than 2.6g/cm3, thermal expansion coefficient≤50 × 10‑7/ DEG C, strain point >=695 DEG C of glass, the physical parameter of glass can satisfy the composition requirements of substrate glasses in the composition range.

Description

A kind of alkali-free silicate glass of low-expansion coefficient high strain-point
[technical field]
The invention belongs to base plate glass field, specially a kind of alkali-free silicate glass of low-expansion coefficient high strain-point.
[background technique]
In recent years, as the demand of Thin Film Transistor-LCD (TFT-LCD) is continuously increased, China is as TFT- The consumption big country of LCD pays more attention to the production of production TFT-LCD substrate used thereof glass.Base plate glass can be used for liquid crystal The electronic devices such as TV, liquid crystal display, laptop, tablet computer and mobile phone, base plate glass is as film display industry Foundation stone, be not only widely used in the liquid crystal panel structures such as TN/STN, TFT and the essential base material of OLED, base Glass sheet importance is influenced limited by display mechanism variation, has irreplaceability, and Mirae Corp. holds a stable position, therefore, base The quality requirements of glass sheet also with market development and be continuously improved；Base plate glass is to constitute the important raw material of liquid crystal display panel One of, the key structure of liquid crystal display panel is similar to sandwich, two layers " bread " (TFT substrate and colored filter) folder " jam " (liquid crystal), therefore make a piece of TFT-LCD panel and need to use two sheet glass, respectively as bottom glass substrate and colored filter Bottom plate uses.Base plate glass accounting about 20% in the TFT-LCD cost of raw material, the influence to panel product performance are very huge Greatly, the indexs such as the resolution ratio, light transmittance of panel finished product, thickness, weight, visible angle are all close with used base plate glass quality Cut phase is closed, and as important base material, base plate glass is very huge for the meaning of TFT-LCD industry.
The performance of glass substrate used in TFT-LCD need to meet following liquid crystal display panel manufacture and require: 1) low-density: for big ruler Very little glass substrate, density is lower, and the weight of glass substrate is lower, is readily transported；2) low thermal coefficient of expansion: the coefficient will determine glass Glass material is because of the ratio of apparent size expansion or shrinkage caused by temperature change, and the lower coefficient the better, so that the heat expansion of large screen Shrinkage reduces to minimum, to guarantee the matching degree of two sheet glass of front and back in manufacturing process；3) alkali-free formula: for TFT-LCD, it is desirable that The manufacture of its substrate must be formulated using alkali-free.Once containing monovalence alkali metal in glass, monovalence alkali metal can be from high temperature Inside glass is overflowed as glass surface, be will affect the stability of thin film transistor (TFT) grid voltage, is caused the short circuit or failure of printed circuit Deng；4) high strain-point: the maximum temperature that substrate needs to be heat-treated repeatedly reaches 625 DEG C, therefore it is required that substrate is at this temperature Keep rigidity, cannot have any viscid flow phenomenon, otherwise not only glass deformation and cooling when bring thermal stress, also will cause The variation of size, therefore the strain point of glass substrate is generally required to be higher than 650 DEG C；5) chemical stability: base plate glass requirement must The various chemical treatments in display production must be stood, as a-Si active matrix, LCD have 7 layers or more of thin film circuit Corrosion step, corrosive agent and cleaning agent strong acid as much to highly basic, such as 10% HF, 5% HCl, 5% NaOH, dense HNO3/ 10% HF-HNO3Deng, it may be said that requirement of the substrate to chemical stability is almost most stringent of in glassware.
And in the prior art, most base plate glass product can satisfy said one to two conditions, it can be difficult to So that the performance of base plate glass can satisfy above-mentioned all demands, the density of such as most of base plate glass is about in 2.3~2.7g/ cm3In range, but its strain point, about within the scope of 600~685 DEG C, the thermal expansion coefficient within the scope of 0~300 DEG C is 35~55 ×10-7/ DEG C within the scope of, if testing within the scope of 30~380 DEG C, thermal expansion coefficient can be higher.
[summary of the invention]
It is an object of the invention to overcome the above-mentioned prior art, a kind of nothing of low-expansion coefficient high strain-point is provided Alkali silicate glass.The glass by limit glass chemical constituent so that the glass have the lower coefficient of expansion and Higher strain point, while the lower chemical stability of density is good；Meet the composition requirements of substrate glasses.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of alkali-free silicate glass of low-expansion coefficient high strain-point, is calculated in mass percent, the no alkali silicate The component of glass are as follows: SiO2: 51.2%~62%；Al2O3: 18.4%~20.5%；B2O3: 4.4%~4.9%；MgO:1.4% ~3%；CaO:6%~8.5%；SrO:3.4%~8.4%；BaO:0.6%~5.6%；SnO2: 0.17%~0.21%.
A further improvement of the present invention is that:
Preferably, it is calculated in mass percent, the component of the alkali-free silicate glass are as follows: SiO2: 55%~62%； Al2O3: 18.4%~20.5%；B2O3: 4.4%~4.9%；MgO:1.4%~3%；CaO:6%~8.5%；SrO:3.4% ~8.4%；BaO:0.6%~5.6%；SnO2: 0.17%~0.21%.
Preferably, SiO2With Al2O3Mass percent summation are as follows: 71%~81.5%.
Preferably, alkaline-earth metal mass percent summation are as follows: 13.9%~24.3%.
Preferably, density≤2.6g/cm of the alkali-free silicate glass3。
Preferably, thermal expansion coefficient≤50 × 10 of the alkali-free silicate glass within the scope of 30 DEG C~380 DEG C-7/℃。
Preferably, strain point >=695 DEG C of the alkali-free silicate glass.
Compared with prior art, the invention has the following advantages:
The invention discloses a kind of alkali-free silicate glasses of low-expansion coefficient high strain-point.The glass defines each oxygen The chemical constituent of compound, wherein the main component SiO of compound2It limits in a certain range, while improving strain point of glass, It ensure that the chemical stabilities such as the acid resistance of glass；Define SiO2With Al2O3Mass percent summation can be improved glass Strain point and elasticity modulus increase the chemical stability of glass.It is substantially free of alkali metal oxide in the glass ingredient, ensure that The stability of thin film transistor (TFT) grid voltage；Glass density in the chemical constituent is lower than 2.6g/cm3, thermal expansion coefficient≤50 × 10-7/ DEG C, strain point >=695 DEG C of glass, the ingredient that the physical parameter of glass can satisfy substrate glasses in the composition range needs It asks.
[specific embodiment]
The invention will be described in further detail combined with specific embodiments below.The invention discloses a kind of low-expansion coefficients The ingredient of the alkali-free silicate glass of high strain-point, is calculated in mass percent, the component of the glass are as follows: SiO2: 51.2%~ 62%；Al2O3: 18.4%~20.5%；B2O3: 4.4~4.9%；MgO:1.4%~3%；CaO:6%~8.5%；SrO: 3.4%~8.4%；BaO:0.6%~5.6%；SnO2: 0.17%~0.21%；Preferably, SiO2Content is 55%~62%； SiO2With Al2O3Mass percent summation range are as follows: 71%~81.5%；The range of alkaline-earth metal mass percent summation Are as follows: 13.9%~24.3%.
Partial materialization performance under this glass ingredient is as follows: density≤2.6g/cm of glass3；Glass is 30 DEG C~380 Thermal expansion coefficient≤50 × 10 in DEG C temperature range-7/℃；Strain point >=695 DEG C of glass.
SiO2It is the main compound to form glass, it is to form irregular company with the structure of oxygen-octahedron [SiO4] Continuous network is the skeleton of glass；Pure SiO2The coefficient of expansion it is very low, be (5~7) × 10-7/℃；Therefore, SiO2It can reduce The thermal expansion coefficient and density of glass, improve the strain point of glass；If SiO2The mouldability of too high levels, glass composition can drop It is low, increase the difficulty that the glass is melted；If but SiO2Content can reduce the chemical stabilities such as the acid resistance of glass when too low, no Easily obtain the glass of low bulk, low-density and high strain-point；Therefore, SiO in the present invention2Content is 51.2%~62%；It is preferred that , SiO2Content is 55%~62%.
Al2O3For intermediate oxide, when O deficiency in glass, the ligancy of Al is 6, is in network gap, is formed with O 【AlO6] octahedra；When there is extra O in glass, the ligancy of Al is 4, into glass network, forms [AlO with O4] four sides Body plays the role of net mending, increases stability, glass, reduces glass expansion coefficient；Simultaneously because [AlO4] tetrahedron volume is larger, Glass density can be reduced.Al2O3The strain point and elasticity modulus that glass can be significantly improved, increase the chemical stability of glass； Al in the present invention2O3Content be 18.4%~20.5%.
On this basis, SiO2With Al2O3Content be it is complementary, the ratio that sum of the two accounts for raw material total amount should be big In 70%；Preferably, SiO2With Al2O3Quality summation in 71%~81.3% range.
B2O3Effect in the glass composition is fluxing agent, it can reduce glass melting viscosity, reduces the thermal expansion of glass Coefficient, suitable B2O3Hydrofluoric acid resistant ability can be increased, and make it easier to process；B2O3Having reduces fusing point and is conducive to melted Effect, but it reduces transition temperature simultaneously, and extremely harmful to chemical durability, and strain point can be too low, therefore B2O3Contain Amount is preferably 10% hereinafter, B in the present invention2O3Content below 5%.
Alkaline earth oxide RO in glass includes MgO, CaO, SrO and BaO, and wherein the mass content of RO is 13.9% In~24.3% range.With the increase of RO ionic radius, the density and thermal expansion coefficient of glass can all be incremented by.MgO is added can To reduce the melting temperature of glass and increase strain point, relatively other several alkaline earth oxides (CaO, SrO, BaO), MgO can reduce thermal expansion coefficient, therefore can make thermal expansion coefficient in controlled range by adjusting the glass of MgO and SrO, BaO. CaO helps to improve the strain point of glass, and the viscosity of glass can be reduced under high temperature, reduces and difficulty is melted, promote melting for glass Change and clarify, but quickly, forming operation is difficult for viscosity increase when temperature reduction；The addition of SrO and BaO can all make the heat of glass swollen Swollen coefficient increases, if SrO too high levels, can reduce the acid resistance and alkali resistance of glass, reduce the resistance to of etchant resist stripper Long property；BaO is tended to reduce melting temperature and is reduced liquidus temperature.Therefore alkaline earth metal content designs such as in the present invention Under: MgO:1.4%~3%；CaO:6%~8.5%；SrO:3.4%~8.4%；BaO:0.6%~5.6%；Preferably, alkali Earth metal mass percent summation are as follows: 13.9%~24.3%.
SnO2, be substitution Toxic arsenic oxide arsenoxide and a kind of raw material as clarifying agent, be conducive to gas in glass melting process The discharge of bubble, but content excessively then calculus easy to form, therefore the SnO in the present invention2Content is less than 0.21%.
Glass ingredient in the present invention is prepared by the following method:
1) it is formed according to the glass of design, carries out selection, calculating, weighing and the mixing of raw material；Raw material includes silica sand, oxidation Aluminium powder, boric acid, boron oxide, magnesia, magnesium carbonate, calcium oxide, calcium carbonate, strontium carbonate, barium carbonate, barium nitrate and tin oxide.
2) uniformly mixed powder is poured into platinum crucible, 3~5h is kept the temperature at 1580 DEG C~1650 DEG C, then will be melted The glass metal made pours into the die for molding having been warmed up；The preheating temperature of mold is 650-750 DEG C.
3) both bulk glasses after molding are put into the annealing furnace for having risen to 650 DEG C~750 DEG C, anneal 30-60min；Again Simple working process, sample needed for being prepared into various tests, with stand-by are carried out to the glass sample after annealing.
The sample prepared tests sample by various standard method of test.
The density that glass is measured according to Archimedes's drainage, is answered according to the annealing point of ASTM C-336 standard testing glass Height tests the resistance to of glass using the method for chemical immersion according to the thermal expansion coefficient CTE of ASTM C-372 standard testing glass Chemical corrosivity.
Embodiment
Embodiment 1:
1. mixed raw material powder is poured into platinum crucible, 4h is kept the temperature at 1630 DEG C, the glass metal melted is poured into The die for molding having been warmed up.
2. both bulk glasses after molding are put into annealing furnace, annealing temperature is 730 DEG C, annealing time 45min；
The glass ingredient obtained under the preparation parameter are as follows: SiO2: 62%；Al2O3: 19.4%；B2O3: 4.57%；MgO: 2.62%；CaO:7.1%；SrO:3.5%；BaO:0.6%；SnO2: 0.21%；According to glass physical parameter made from the ingredient It is as follows: density 2.47g/cm3；Thermal expansion coefficient: 36.77 × 10-7/℃；715 DEG C of strain point；Resistant to chemical etching/mass loss, HCl 5%-95 DEG C-is for 24 hours: 0.25mg/cm2；NH4F:HF-10%-20 DEG C of -20min:1.14mg/cm2；HF-10%-20 DEG C- 20min:5.1mg/cm2；NaOH-95 DEG C of -6h:1.43mg/cm2。
Table 1 is the remaining embodiment in the present invention, and (table 1-1 is embodiment 2-5, and table 1-2 is embodiment 6-10) is according to setting The melted preparation that component carries out sample is counted, the glass within the scope of present component is obtained, density is carried out to the sample after being melted, The test of thermal expansion coefficient and strain point；(table 2-1 is embodiment to the corresponding preparation process technological parameter of each embodiment of table 2 2-5, table 2-2 are embodiment 6-10).
Table 1-1 glass combination chemical constituent and its correspondence physical parameter (embodiment 2-5)
Table 1-2 glass combination chemical constituent and its correspondence physical parameter (embodiment 6-10)
Table 2-1 manufacturing parameter (embodiment 2-5)
Table 2-2 manufacturing parameter (embodiment 6-10)
Embodiment 6 7 8 9 10
Crucible temperature/DEG C 1650 1630 1630 1630 1620
Soaking time/h 5 4 3 3 4
Annealing temperature/DEG C 750 720 700 700 680
Annealing time/min 50 30 50 50 60
Ingredient design of the invention and preparation process are mainly while meeting the following demand of TFT-LCD glass substrate: 1. low-density: for TFT-LCD, LCD TV and notebook computer are current biggest market, therefore the glass substrate Density is the smaller the better, because weight can be increasing, and designs it from ingredient with the continuous increase of glass substrate size Small density, can convenient for the transport in manufacturing process, and be made after finished product special mountings such as suspension on the wall, equipment transport and Carry etc.；2. thermal expansion coefficient: the coefficient will determine glass material because of the ratio of apparent size expansion or shrinkage caused by temperature change Example, the lower coefficient the better, so that expanding with heat and contract with cold for large screen reduces to minimum, to guarantee two sheet glass of front and back in manufacturing process Matching degree.On the other hand, due to display in the fabrication process will by repeatedly, repeatedly, rapidly heating cooling, necessarily cause Glass structure relaxation, occurs change in size, and deviation occurs in the electronic circuit that can thus make photoetching make a plate, it requires entire base The contraction size of panel element can only be the part of the most thin width in circuit diagram, i.e., several microns, low thermal contraction is still It is necessary condition, in general, the coefficient of expansion of base plate glass is in 0~300 DEG C of temperature range less than 40 × 10-7/ DEG C；③ The limitation of alkali metal: for TFT-LCD, it is desirable that the manufacture of its substrate must be formulated using alkali-free.Because being printed on base plate glass The requirement of brush circuit, glass cannot contain monovalence alkali metal, i.e. R2O content is low as far as possible, and even zero.Once containing in glass There is monovalence alkali metal, monovalence alkali metal can be overflowed from inside glass as glass surface at high temperature, will affect thin film transistor (TFT) grid The stability of pressure causes short circuit or failure of printed circuit etc., therefore, forbids monovalence alkali metal ion in liquid crystal substrate glass Appearance；4. strain point: in manufacture TFT technical process, substrate needs heat treatment repeatedly, and temperature highest will be heated to 625 DEG C, it is desirable that substrate keeps rigidity at this temperature, cannot have any viscid flow phenomenon, otherwise not only glass deformation and cooling When bring thermal stress, also will cause the variation of size.Therefore it is required that the strain point of glass substrate is higher than 625 DEG C, 25 are added DEG C insurance amount, the strain point of glass at least will be at 650 DEG C or more；5. chemical stability: base plate glass requires to stand Various chemical treatments in display production, as a-Si active matrix, LCD have 7 layers or more of thin film circuit and as much Corrosion step, corrosive agent and cleaning agent strong acid to highly basic, such as 10% HF, 5% HCl, 5% NaOH, dense HNO3/10% HF-HNO3 etc., it may be said that requirement of the substrate to chemical stability is almost most stringent of in glassware.
In conjunction with the above-mentioned requirement to glass substrate and table 1, it can be seen that the corresponding physics of glass ingredient within this range Performance: density≤2.6g/cm of glass3While, strain point >=695 DEG C of glass, and glass is in 30 DEG C~380 DEG C temperature models Enclose interior thermal expansion coefficient≤50 × 10-7/℃；The comprehensive physical performance of glass is better than existing major part in this composition range Base plate glass.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (7)

1. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point, which is characterized in that be calculated in mass percent, the nothing The component of alkali silicate glass are as follows: SiO2: 51.2%~62%；Al2O3: 18.4%~20.5%；B2O3: 4.4%~4.9%； MgO:1.4%~3%；CaO:6%~8.5%；SrO:3.4%~8.4%；BaO:0.6%~5.6%；SnO2: 0.17%~ 0.21%.
2. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point according to claim 1, which is characterized in that with Mass percentage, the component of the alkali-free silicate glass are as follows: SiO2: 55%~62%；Al2O3: 18.4%~20.5%； B2O3: 4.4%~4.9%；MgO:1.4%~3%；CaO:6%~8.5%；SrO:3.4%~8.4%；BaO:0.6%~ 5.6%；SnO2: 0.17%~0.21%.
3. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point according to claim 1, which is characterized in that SiO2With Al2O3Mass percent summation are as follows: 71%~81.5%.
4. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point according to claim 1, which is characterized in that alkali Earth metal mass percent summation are as follows: 13.9%~24.3%.
5. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point according to claim 1, which is characterized in that institute State density≤2.6g/cm of alkali-free silicate glass3。
6. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point according to claim 1, which is characterized in that institute State thermal expansion coefficient≤50 × 10 of the alkali-free silicate glass within the scope of 30 DEG C~380 DEG C-7/℃。
7. a kind of alkali-free silicate glass of low-expansion coefficient high strain-point described in -6 any one according to claim 1, It is characterized in that, strain point >=695 DEG C of the alkali-free silicate glass.
CN201810844721.9A 2018-07-27 2018-07-27 A kind of alkali-free silicate glass of low-expansion coefficient high strain-point Pending CN108947237A (en)

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Application publication date: 20181207