CN105731790A - Alkali-free aluminosilicate glass, composition for same, method for preparing alkali-free aluminosilicate glass and application thereof - Google Patents
Alkali-free aluminosilicate glass, composition for same, method for preparing alkali-free aluminosilicate glass and application thereof Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 38
- 239000005354 aluminosilicate glass Substances 0.000 title abstract 7
- 239000011521 glass Substances 0.000 claims abstract description 108
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 18
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 16
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 13
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 13
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005368 silicate glass Substances 0.000 claims description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 15
- 230000003628 erosive effect Effects 0.000 claims description 13
- 230000004927 fusion Effects 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 8
- 238000005260 corrosion Methods 0.000 claims description 8
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 4
- 239000003518 caustics Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 15
- 238000005516 engineering process Methods 0.000 abstract description 12
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- -1 mechanical strength Substances 0.000 description 4
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 3
- 238000004031 devitrification Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000004293 potassium hydrogen sulphite Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- 229910001637 strontium fluoride Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
- G09F9/35—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements being liquid crystals
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Theoretical Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Optics & Photonics (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to the field of technologies for producing glass, and discloses alkali-free aluminosilicate glass, a composition for the same, a method for preparing the alkali-free aluminosilicate glass and application thereof. The composition for the alkali-free aluminosilicate glass comprises, by weight in oxide, 63-72wt% of SiO2, 15-20wt% of Al2O3, 4-10wt% of MgO, 2-6wt% of CaO, 0.01-2.5wt% of SrO, 2-8wt% of BaO, 0.1-1.5wt% of In2O3 and 0.1-0.3wt% of SnO2. The alkali-free aluminosilicate glass, the composition, the method and the application have the advantages that the alkali-free aluminosilicate glass is high in strain point, chemical stability, Young modulus and transmittance, low in melting temperature, expansion coefficient, density and liquid-phase linear temperature and particularly applicable to TFT-LCD (thin film transistor-liquid crystal display) and OLED (organic light emitting diode) glass substrates with low-temperature poly-silicon (LTPS) technologies.
Description
Technical field
The present invention relates to field of glass production technology, in particular it relates to a kind of alkali-free alumina silicate glass compositions, nothing
Alkali alumina silicate glass and its preparation method and application.
Background technology
Low temperature polycrystalline silicon (Low Temperature Poly-silicon is called for short LTPS) is a new generation's membrane transistor liquid
With the maximum difference of tradition amorphous silicon displays, the manufacturing process of crystal display (TFT-LCD), is that it has high-resolution, anti-
Answer the advantages such as speed fast, high brightness, high aperture, add the silicon crystalline arrangement relatively a-Si orderliness due to LTPS-TFT LCD,
Make relatively high more than 100 times of electron mobility, peripheral drive circuit can be made on the glass substrate simultaneously, reach system
Target, saving space and the cost of driving IC integrated.Along with fast development and the portable electronic of flat panel display produce
Popularizing rapidly of product such as notebook computer, panel computer, smart mobile phone and Intelligent worn device, liquid crystal display is played the part of wherein
Role more and more important, there is lcd products more market lightening, high-res, high image quality and accepted.
Low temperature polycrystalline silicon TFT needs the most repeatedly to process in the fabrication process, and substrate must be at multiple high temp
Can not deform in processing procedure, base plate glass performance is just had higher requirement by this, and preferred strain point is higher than 650
DEG C, more preferably above 670 DEG C, 700 DEG C, 720 DEG C, 740 DEG C, so that substrate has the least heat receipts in panel processing procedure
Contracting, therefore the strain point temperature of substrate is the highest more good.The thermal coefficient of expansion of glass substrate needs the thermal coefficient of expansion with silicon simultaneously
Close, reduce stress and destruction as far as possible, therefore the preferred thermal linear expansion coefficient of base plate glass is 28 × 10-7/℃-39×
10-7/ DEG C between.For the ease of producing, reducing production cost, the glass as display base plate should have relatively low fusing
Temperature and liquidus temperature.But most of silicate glass high temperature viscosities and low temperature viscosity can keep close speedup, along with
LTPS technology more and more higher to thermal stability requirement (high strain point), often there is constant amplitude, is even significantly increased in high temperature viscosity.
Under existing refractory technology and cell furnace production technology premise, the every bit increase of high temperature viscosity is all to glass production
The significant challenge of technology.As, in existing amorphous silicon glass substrate production technique, fusion temperature is often beyond 1550 DEG C, even
1600 DEG C, more even 1650 DEG C, along with the lifting of glass melting temperature, vitreous humour and volatile matter thereof are to refractory material and platinum device
Erosion rate is that geometry multiple increases, and brings two catastrophic consequences: one is that defect is increased sharply, and yield is had a greatly reduced quality；Two is to produce
The line life-span significantly shortens, and is all serious disaster from investment and environmental angle.Along with glass substrate is claimed by LTPS technology
Raising, how improving low temperature viscosity, (viscosity is more than 107Moor above region, i.e. temperature less than softening point area below)
Effectively reduce high temperature viscosity simultaneously and become the major tasks of LTPS glass technology research and development.
Summary of the invention
The invention aims to overcome drawbacks described above of the prior art, it is provided that a kind of alkali-free alumina silicate glass is used
Compositions, alkali-free alumina silicate glass and its preparation method and application.
To achieve these goals, first aspect, the invention provides a kind of alkali-free alumina silicate glass compositions, with
On the basis of the weight of said composition, in terms of oxide, said composition contains the SiO of 63-72wt%2, the Al of 15-20wt%2O3、
The In of BaO, 0.1-1.5wt% of SrO, 2-8wt% of CaO, 0.01-2.5wt% of MgO, 2-6wt% of 4-10wt%2O3With
The SnO of 0.1-0.3wt%2。
Under preferable case, by weight percentage, MgO/RO > 0.4, wherein, RO=MgO+CaO+SrO+BaO.
Under preferable case, by weight percentage, SiO2+Al2O3> 83wt%.
Under preferable case, on the basis of the weight of said composition, In2O3Content be 0.5-1.2wt%.
Under preferable case, on the basis of the weight of said composition, the content of MgO is 5-8wt%.
Under preferable case, on the basis of the weight of said composition, the content of BaO is 3.5-7.5wt%.
Under preferable case, on the basis of the weight of said composition, Al2O3Content be 16-18.5wt%.
Under preferable case, on the basis of the weight of said composition, SnO2Content be 0.15-0.25wt%.
Under preferable case, on the basis of the weight of said composition, the content of CaO is 3-5.5wt%.
Under preferable case, described compositions possibly together with clarifier, described clarifier more preferably sulfate, nitric acid
At least one in salt, chloride and fluoride；On the basis of the weight of said composition, the content of clarifier is not more than 1wt%.
Second aspect, the invention provides a kind of method preparing alkali-free alumina silicate glass, and the method includes this
Bright described alkali-free alumina silicate glass compositions carries out melt process, forming processes, annealing and machining successively
Process.
The third aspect, the invention provides the alkali-free alumina silicate glass that said method prepares.
Under preferable case, the strain point of described alkali-free alumina silicate glass is not less than 740 DEG C, and fusion temperature is less than 1620
DEG C, liquidus temperature is less than 1150 DEG C, and the thermal coefficient of expansion in the range of 50-350 DEG C is 30 × 10-7/℃-38×10-7/ DEG C, close
Degree is not more than 2.47g/cm3, at 24 ± 0.5 DEG C, the erosion amount of the HF solution acid corrosion 20min of 5wt% is not more than 3mg/cm2, 90
At ± 5 DEG C, the erosion amount of the NaOH solution caustic corrosion 20h of 5wt% is not more than 0.5mg/cm2, it is seen that light transmission rate is higher than 91%,
Young's modulus is higher than 80GPa.
Fourth aspect, the invention provides alkali-free alumina silicate glass compositions of the present invention or alkali-free aluminum silicate
The application in preparing display device and/or photoelectric device of the salt glass, be preferably preparation TFT-LCD glass substrate and/or
Application in OLED glass substrate.
The alkali-free alumina silicate glass compositions of the present invention, is the material side of a kind of environmental type glass, can be with overflowing
Flow down traction therapy and produce into glass substrate.The glass prepared has higher strain point, relatively low fusion temperature, relatively low swollen
Swollen coefficient, higher chemical stability and mechanical performance, higher Young's modulus, higher transmitance, relatively low density and relatively
Low liquidus temperature (the In in formula composition2O3, MgO there is reduction glass high temperature viscosity and do not reduce low temperature viscosity, improvement
The effect of chemical durability of glass), meet the development trend of flat panel display, be particularly well-suited to low temperature polycrystalline silicon LTPS technology
TFT-LCD, OLED glass substrate.
A preferred embodiment of the invention, in alkali-free alumina silicate glass compositions, with percentage by weight
Meter, MgO/RO > 0.4 (RO=MgO+CaO+SrO+BaO), SiO2+Al2O3> 83wt% time, in terms of oxide, glass compositions
In containing the SiO of certain content2、Al2O3、MgO、CaO、SrO、BaO、In2O3And SnO2, utilize this glass compositions to be prepared into
The glass arrived, what its physical characteristic can be stable reaches: strain point is not less than 740 DEG C, and fusion temperature is less than 1620 DEG C, liquidus curve
Temperature is less than 1150 DEG C, and the thermal coefficient of expansion in the range of 50-350 DEG C is 30 × 10-7/℃-38×10-7/ DEG C, density is not more than
2.47g/cm3, in concentration is 5wt%HF solution, at 24 ± 0.5 DEG C, corroding 20min, erosion amount is not more than 3.0mg/cm2；?
Concentration is in 5wt%NaOH solution, corrodes 20h at 90 ± 5 DEG C, and erosion amount is not more than 0.5mg/cm2；Through 5wt%HF solution,
Glass surface after the erosion of 5wt%NaOH solution is all without the bad deficient point such as " pit ", " sags and crests ", it is seen that light transmission rate is higher than
91%, Young's modulus is higher than 80GPa.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that described herein specifically
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
In the present invention, it will be understood by those skilled in the art that " alkali-free " to refer in glass composition or glass not contain
Alkali metal (i.e. six alkali metals of group ia in the periodic table of elements).
First aspect, the invention provides a kind of alkali-free alumina silicate glass compositions, with the weight of said composition is
Benchmark, in terms of oxide, said composition contains the SiO of 63-72wt%2, the Al of 15-20wt%2O3, MgO, 2-of 4-10wt%
The In of BaO, 0.1-1.5wt% of SrO, 2-8wt% of CaO, 0.01-2.5wt% of 6wt%2O3With 0.1-0.3wt%'s
SnO2。
The present inventor under study for action it has furthermore been found that by weight percentage, during MgO/RO > 0.4, wherein, RO
=MgO+CaO+SrO+BaO, it is possible to improve the combination property of the glass prepared further, improve strain point, reduction liquid phase
Line temperature also improves chemical stability.Therefore, in order to improve the combination property of the glass prepared further, improve strain
Point, reduce liquidus temperature and improve chemical stability, under preferable case, by weight percentage, MgO/RO > 0.4, wherein,
RO=MgO+CaO+SrO+BaO.
The present inventor under study for action it has furthermore been found that by weight percentage, SiO2+Al2O3> 83wt% time, energy
Enough improve the glass prepared further combination property, improve strain point, reduce liquidus temperature and improve chemically stable
Property.Therefore, in order to improve the combination property of the glass prepared further, improve strain point, reduction liquidus temperature and carry
High chemical stability, under preferable case, by weight percentage, SiO2+Al2O3> 83wt%.
In the glass compositions of the present invention, SiO2Being glass former, content is too low, is easily caused strain point and reduces, heat
The coefficient of expansion increases, and acid resistance, alkali resistance decline；Improve SiO2Content can reduce the thermal coefficient of expansion of glass, improves glass
Heat stability, the performance such as chemical stability, but fusion temperature raises, and general kiln is difficult to meet, and may cause analysis
Brilliant.Therefore, consider, on the basis of the weight of said composition, in terms of oxide, SiO2Content be 63-72wt%.
In the glass compositions of the present invention, Al2O3Belong to intermediate oxide, in order to improve the intensity of glass structure, if
Content is less than 15wt%, the easy devitrification of glass, is also easily subject to extraneous aqueous vapor and the erosion of chemical reagent.The Al of high-load2O3Have
Help the raising of strain point of glass, mechanical strength, chemical stability, but crystallization easily occurs in too high glass, can make simultaneously
Obtain glass to be difficult to dissolve.Therefore, consider, on the basis of the weight of said composition, in terms of oxide, Al2O3Content be
15-20wt%, preferably 16-18.5wt%.
In the glass compositions of the present invention, MgO is network modifying oxide, it is possible to increase chemical durability of glass and fall
Low high temperature viscosity.But if content of MgO is more than 10wt%, glass endurance can be deteriorated, simultaneously the easy devitrification of glass.Therefore, combine
Closing and consider, on the basis of the weight of said composition, in terms of oxide, the content of MgO is 4-10wt%, preferably 5-8wt%.
In the glass compositions of the present invention, CaO is network modifying oxide, can reduce the viscosity of glass when high temperature,
Promoting the fusing of glass and clarification, but when content is higher, the crystallization tendency of glass can be made to increase, thermal coefficient of expansion also can amplitude variation greatly
Greatly.Therefore, considering, on the basis of the weight of said composition, in terms of oxide, CaO content is 2-6wt%, preferably 3-
5.5wt%.
In the glass compositions of the present invention, SrO can improve the chemical stability of glass and accelerate glass melting, but contains
Clarification can be made when measuring too high secondary bubble occur, and also resulting in glass density increases.Therefore, consider, with said composition
On the basis of weight, in terms of oxide, SrO content is 0.01-2.5wt%.
In the glass compositions of the present invention, BaO is for reducing the viscosity of glass and promoting the melted of glass and prevent glass
There is crystallize in glass, if content is too much, glass density can be caused to increase.Therefore, consider, with the weight of said composition as base
Standard, in terms of oxide, BaO content is 2-8wt%, preferably 3.5-7.5wt%.Wherein, in said composition, with said composition
On the basis of weight, the incorporation way of BaO is BaCO3、BaSO4With Ba (NO3)2In at least one, and in terms of BaO, BaSO4With/
Or Ba (NO3)2Content be 0.1-2.5wt%.BaSO4Silicate reaction process can be effectively facilitated and reduce pyrometric scale surface tension,
Cause alveolar layer to seethe at tank furnace material mountain back segment to change with partial pressure, effectively facilitate fusing and clarifying process.
In the glass compositions of the present invention, In2O3For network modifying oxide, there is the viscosity reducing glass, improve glass
The effect of glass strain point, endurance and dielectric properties, and can substantially reduce glass surface tension.But too high levels has increase glass
The density of glass and the effect of refractive index, In2O3It is unfavorable when content is more than 1.5% to stablize devitrification of glass, and affects the saturating of glass
Cross rate.Therefore, consider, on the basis of the weight of said composition, in terms of oxide, In2O3Content be 0.1-1.5wt%,
It is preferably 0.5-1.2wt%.
In the glass compositions of the present invention, on the basis of the weight of said composition, in terms of oxide, SnO2Content be
0.1-0.3wt%, preferably 0.15-0.25wt%.
It will be understood by those skilled in the art that in the alkali-free alumina silicate glass compositions of the present invention, compositions
Containing SiO2、Al2O3、MgO、CaO、SrO、BaO、In2O3And SnO2Refer to that said composition contains containing Si compound, containing Al chemical combination
Thing, containing Mg compound, containing Ca compound, containing Sr compound, containing Ba compound, containing In compound and the compound Han Sn, as containing front
State the carbonate of each element, nitrate, sulfate, oxide etc., and the content of the aforementioned each component mentioned is all with each element
Oxide meter, the concrete carbonate of each element, nitrate, sulfate, oxide to be chosen as those skilled in the art institute ripe
Know, do not repeat them here.
In the glass compositions of the present invention, according to the difference of glass preparation technique, compositions can also be containing as glass
Clarifier when glass melts, described clarifier is preferably at least one in sulfate, nitrate, chloride and fluoride；With
On the basis of the weight of said composition, the content of clarifier is not more than 1wt%.Specifically chosen for clarifier the most particularly limits
Fixed, can be various selections commonly used in the art, such as sulfate can be barium sulfate, nitrate can be strontium nitrate and/or
Barium nitrate, chloride can be barium chloride and/or strontium chloride, and fluoride can be calcium fluoride.
In the glass compositions of the present invention, when utilizing it to prepare alkali-free alumina silicate glass, why enable to glass
Glass has aforementioned excellent combination property, is mainly attributed to cooperating between each component, especially SiO in compositions2、
Al2O3、MgO、CaO、SrO、BaO、In2O3And SnO2Between mating reaction, each component of the most aforementioned certain content it
Between cooperate.
Second aspect, the invention provides a kind of alkali-free alumina silicate glass, on the basis of the weight of described glass, described
Glass contains the SiO of 63-72wt%2, the Al of 15-20wt%2O3, CaO, 0.01-of MgO, 2-6wt% of 4-10wt%
The In of BaO, 0.1-1.5wt% of SrO, 2-8wt% of 2.5wt%2O3SnO with 0.1-0.3wt%2。
Preferably, in alkali-free alumina silicate glass, by weight percentage, MgO/RO > 0.4, wherein, RO=MgO+CaO+
SrO+BaO。
Preferably, in alkali-free alumina silicate glass, by weight percentage, SiO2+Al2O3> 83wt%.
Preferably, in alkali-free alumina silicate glass, on the basis of the weight of described glass, In2O3Content be 0.5-
1.2wt%.
Preferably, in alkali-free alumina silicate glass, on the basis of the weight of described glass, the content of MgO is 5-8wt%.
Preferably, in alkali-free alumina silicate glass, on the basis of the weight of described glass, the content of BaO is 3.5-
7.5wt%.
Preferably, in alkali-free alumina silicate glass, on the basis of the weight of described glass, Al2O3Content be 16-
18.5wt%.
Preferably, in alkali-free alumina silicate glass, on the basis of the weight of described glass, SnO2Content be 0.15-
0.25wt%.
Preferably, in alkali-free alumina silicate glass, on the basis of the weight of described glass, the content of CaO is 3-
5.5wt%.
The third aspect, the invention provides a kind of method preparing alkali-free alumina silicate glass, and the method includes this
Bright described alkali-free alumina silicate glass compositions carries out melt process, forming processes, annealing and machining successively
Process.
In the method for the present invention, the concrete restriction for glass compositions refers to the description of aforementioned corresponding contents, at this
Repeat no more.
In the case of process of the present invention it is preferred, the condition of melt process includes: temperature is less than 1650 DEG C, and the time is more than
1h.According to practical situation, those skilled in the art can determine that concrete melt temperature and melting time are (if temperature is 1550-
1650 DEG C, the time is 8-12h), this is well known to those skilled in the art, and does not repeats them here.
In the case of process of the present invention it is preferred, the condition of annealing includes: temperature is 650-800 DEG C, and the time is more than
0.1h.Those skilled in the art can determine concrete annealing temperature and annealing time according to practical situation, and this is this area skill
Known to art personnel, do not repeat them here.
In the method for the present invention, for machining processes, there is no particular limitation, can be common various in this area
Machining mode, can be such as the product that annealing is obtained carry out cutting, grind, polishing etc..
Fourth aspect, the invention provides the alkali-free alumina silicate glass that said method prepares.
It will be understood by those skilled in the art that in the alkali-free alumina silicate glass of the present invention, with the weight of glass be
Benchmark, containing the SiO of 63-72wt%2, the Al of 15-20wt%2O3, CaO, 0.01-of MgO, 2-6wt% of 4-10wt%
The In of BaO, 0.1-1.5wt% of SrO, 2-8wt% of 2.5wt%2O3SnO with 0.1-0.3wt%2。
The preferred scope of the content of concrete each oxide, refers to aforementioned corresponding contents and describes, do not repeat them here.
Under preferable case, the alkali-free alumina silicate glass of the present invention, strain point is not less than 740 DEG C, and fusion temperature is less than
1620 DEG C, liquidus temperature is less than 1150 DEG C, and the thermal coefficient of expansion in the range of 50-350 DEG C is 30 × 10-7/℃-38×10-7/
DEG C, density is not more than 2.47g/cm3, at 24 ± 0.5 DEG C, the erosion amount of the HF solution acid corrosion 20min of 5 weight % is not more than
3mg/cm2, at 90 ± 5 DEG C, the erosion amount of the NaOH solution caustic corrosion 20h of 5 weight % is not more than 0.5mg/cm2, it is seen that light transmission
Rate is higher than 91%, and Young's modulus is higher than 80GPa.
5th aspect, the invention provides alkali-free alumina silicate glass compositions of the present invention or alkali-free aluminum silicate
The application in preparing display device and/or photoelectric device of the salt glass, be preferably preparation TFT-LCD glass substrate and/or
Application in OLED glass substrate.
Embodiment
Hereinafter will be described the present invention by embodiment.In following example, if no special instructions, used
Each material all can be by commercially available, and if no special instructions, method used is the conventional method of this area.
In following example and comparative example, measuring glass density according to Archimedes method, unit is g/cm3。
Use the thermal expansion coefficient of glass of horizontal expander instrument mensuration 50-350 DEG C with reference to ASTM E-228, unit is 10-7/
℃。
Using material mechanical test machine to measure glass Young's modulus with reference to ASTM C-623, unit is GPa.
Bent beam high-temperature viscosimeter is used to measure strain point of glass (10 with reference to ASTM C-33614.5Dpa s strain point
Tst), unit is DEG C.
Use cartridge type to rotate high-temperature viscosimeter with reference to ASTM C-965 and measure the fusion temperature (10 of glass2Dpa s melts
Temperature Tm), unit is DEG C.
Using temperature gradient furnace method to measure vitreous humour liquidus temperature with reference to ASTM C-829, unit is DEG C.
5wt%HF solution (24 ± 0.5 DEG C/20min) and 5wt%NaOH solution (90 ± 5 DEG C/20h) is used to measure glass
Chemical resistance, unit is mg/cm2。
Visible light transmittance rate uses UV-2550 ultraviolet-visible spectrophotometer to measure, and unit is %.
Embodiment 1-8
(wherein, the introducing form of BaO is BaCO to form each component of weighing according to the glass shown in table 13, the content of BaO is
BaCO3Content in terms of BaO), mixing, compound is poured in platinum crucible, in 1620 DEG C of high temperature furnaces, then heat 10 little
Time, and use platinum rod to stir to discharge bubble.The vitreous humour melted is poured in rustless steel cast iron grinding tool, is configured to rule
Fixed both bulk glasses goods, then by glass in the lehr, anneal 2 hours for 760 DEG C, close power supply furnace cooling to 25
℃.Carry out glass cutting, grind, polish, then clean up with deionized water and dry, prepare glass finished-product.Point
The other various performances to each glass finished-product are measured, and the results are shown in Table 1.
Table 1
Embodiment 9-16
According to the method for embodiment 6, except for the difference that, compound composition (corresponding glass composition) and the performance of product that obtains
Measurement result is shown in Table 2.
Table 2
Comparative example 1-2
According to the method for embodiment 6, except for the difference that, compound composition (corresponding glass composition) and the performance of product that obtains
Measurement result is shown in Table 3.
Table 3
Data in table 1-2 and table 3 being compared and understand, the glass that the present invention prepares has significantly higher strain
Point, relatively low fusion temperature, relatively low liquidus temperature and the most preferable chemical stability.
Embodiment 15 in embodiment 6 in table 1 and table 2 is compared and understands, MgO/RO > 0.4, wherein, RO=MgO+CaO+SrO
During+BaO, it is possible to improve the combination property of the glass material prepared further, and improve strain point, reduce liquidus temperature
With raising chemical stability.
Embodiment 16 in embodiment 6 in table 1 and table 2 is compared and understands, by weight percentage, SiO2+Al2O3> 83wt%
Time, it is possible to improve the combination property of the glass material prepared further, and improve strain point, reduce liquidus temperature and carry
High chemical stability.
The method of the present invention utilizes the SiO containing certain content2、Al2O3、MgO、CaO、SrO、BaO、In2O3And SnO2's
Glass prepared by glass compositions, especially when in glass compositions, by weight percentage, MgO/RO > 0.4 (RO=
MgO+CaO+SrO+BaO)、SiO2+Al2O3> 83wt% time, strain point is not less than 740 DEG C, fusion temperature be less than 1620 DEG C, liquid phase
Line temperature is less than 1150 DEG C, and the thermal coefficient of expansion in the range of 50-350 DEG C is 30 × 10-7/℃-38×10-7/ DEG C, density is little
In 2.47g/cm3, at 24 ± 0.5 DEG C, the erosion amount of the HF solution acid corrosion 20min of 5 weight % is not more than 3mg/cm2, 90 ± 5 DEG C
The erosion amount of the NaOH solution caustic corrosion 20h of lower 5 weight % is not more than 0.5mg/cm2, it is seen that light transmission rate is higher than 91%, Young
Modulus is higher than 80GPa.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the technology concept of the present invention, technical scheme can be carried out multiple simple variant, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention, at not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy illustrates the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. an alkali-free alumina silicate glass compositions, it is characterised in that on the basis of the weight of said composition, with oxide
Meter, said composition contains the SiO of 63-72wt%2, the Al of 15-20wt%2O3, 4-10wt% MgO, 2-6wt% CaO,
The In of BaO, 0.1-1.5wt% of SrO, 2-8wt% of 0.01-2.5wt%2O3SnO with 0.1-0.3wt%2。
Compositions the most according to claim 1, it is characterised in that by weight percentage, MgO/RO > 0.4, wherein, RO
=MgO+CaO+SrO+BaO.
Compositions the most according to claim 1, it is characterised in that by weight percentage, SiO2+Al2O3> 83wt%.
Compositions the most according to claim 1, it is characterised in that on the basis of the weight of said composition, In2O3Content
For 0.5-1.2wt%.
5., according to the compositions described in claim 1 or 4, it is characterised in that on the basis of the weight of said composition, MgO contains
Amount is 5-8wt%；
Preferably, on the basis of the weight of said composition, the content of BaO is 3.5-7.5wt%；
Preferably, on the basis of the weight of said composition, Al2O3Content be 16-18.5wt%；
Preferably, on the basis of the weight of said composition, SnO2Content be 0.15-0.25wt%；
Preferably, on the basis of the weight of said composition, the content of CaO is 3-5.5wt%.
Compositions the most according to claim 1, it is characterised in that described compositions possibly together with clarifier, described clarifier
It is preferably at least one in sulfate, nitrate, chloride and fluoride；On the basis of the weight of said composition, clarifier
Content be not more than 1wt%.
7. the method preparing alkali-free alumina silicate glass, it is characterised in that the method includes any in claim 1-6
One described alkali-free alumina silicate glass compositions carries out melt process, forming processes, annealing and machinery successively and adds
Work processes.
8. the alkali-free alumina silicate glass that the method described in claim 7 prepares.
Alkali-free alumina silicate glass the most according to claim 8, it is characterised in that answering of described alkali-free alumina silicate glass
Height is not less than 740 DEG C, and fusion temperature is less than 1620 DEG C, and liquidus temperature is less than 1150 DEG C, and the heat in the range of 50-350 DEG C is swollen
Swollen coefficient is 30 × 10-7/℃-38×10-7/ DEG C, density is not more than 2.47g/cm3, the HF solution acid of 5wt% at 24 ± 0.5 DEG C
The erosion amount of corrosion 20min is not more than 3mg/cm2, at 90 ± 5 DEG C, the erosion amount of the NaOH solution caustic corrosion 20h of 5wt% is little
In 0.5mg/cm2, it is seen that light transmission rate is higher than 91%, and Young's modulus is higher than 80GPa.
10. in claim 1-6 described in alkali-free alumina silicate glass compositions described in any one or claim 8 or 9
Alkali-free alumina silicate glass application in preparing display device and/or photoelectric device, be preferably at preparation TFT-LCD glass
Application in substrate and/or OLED glass substrate.
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| CN109231816A (en) * | 2018-10-09 | 2019-01-18 | 成都中光电科技有限公司 | A kind of glass substrate and preparation method thereof can be used for LTPS |
| CN112441743A (en) * | 2020-11-26 | 2021-03-05 | 河南旭阳光电科技有限公司 | Alkali-free glass composition, alkali-free glass, preparation method and application |
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