CN101913764A - Alkali-free alumina silicate glass with high strain point - Google Patents
Alkali-free alumina silicate glass with high strain point Download PDFInfo
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- CN101913764A CN101913764A CN 201010237514 CN201010237514A CN101913764A CN 101913764 A CN101913764 A CN 101913764A CN 201010237514 CN201010237514 CN 201010237514 CN 201010237514 A CN201010237514 A CN 201010237514A CN 101913764 A CN101913764 A CN 101913764A
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- high strain
- point
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Abstract
The invention relates to alkali-free alumina silicate glass with a high strain point, which comprises the following chemical components: 55-70 wt.% of SiO2, 15-25 wt.% of Al2O3, 2-11 wt.% of CaO, 1-6 wt.% of SrO, 3-10 wt.% of ZnO and 1-7 wt.% of ZrO2. The glass does not contain alkali metal oxides, heavy metal oxides, boron oxide or hazardous elements and has the advantages of high strain point, low expansion coefficient, high modulus of elasticity, low founding temperature and the like, is suitable to substrate glass of an SOC (System on Glass), especially suitable to substrate glass for a panel display.
Description
Technical field
The present invention relates to a kind of have high strain-point, low-expansion coefficient, high elastic coefficient, alkali-free metal oxide, the alkali-free alumina silicate glass of oxygen-free boron, it is suitable for preparing the SOG base plate glass; The present invention relates to a kind of flat-panel monitor base plate glass.
Background technology
Liquid-crystal display has driving voltage and low in energy consumption, advantages such as volume is little, light weight, has become the mainstream technology of flat-panel monitor.In lcd technology, low temperature polycrystalline silicon (LTPS, LowTemperature Poly-Silicon) is the manufacturing process of Thin Film Transistor-LCD of new generation (TFT-LCD), the LTPS technology allows the profile of mobile electronic device is more frivolous, with better function, indicating meter is brighter, speed of response is faster, but the preparation temperature of common polycrystalline silicon preparing process can be higher than 600 ℃, and common glass substrate can not be suitable in this case.Some processing in the electron device manufacturings such as liquid-crystal display are included in the technological process of carrying out under the excessive temperature, for example use the active part of thin film transistor and so on to obtain higher response speed in each pixel of TFT-LCD, and low temperature polycrystalline silicon has very high drive current and electronic mobility, therefore the time of response that can improve pixel; In addition, can adopt low temperature polycrystalline silicon technology, directly on glass substrate, make up circuit of display driving, be so-called glass integrated system (SOG, System on Glass), the glass integrated system refers to and electronic component directly is integrated on glass, and polysilicon process will be operated under 800 ℃ temperature at least efficiently, but the thermal expansivity (38 * 10 of its thermal expansivity and silicon
-7/ ℃) can not mate.For other electron devices, conventional treatment step also needs the glass substrate of ability pyroprocessing.The glass that therefore, need have following characteristic:
(1) has high strain-point;
(2) has the thermal expansivity that is complementary with silicon;
(3) has suitable glass smelting temperature;
(4) described glass has good transparently to visible radiation, has good chemical stability.
But up to the present, there is not glass substrate can be applicable to low temperature polycrystalline silicon (LTPS, LowTemperature Poly-Silicon) technology fully as yet, is applied to the base plate glass of glass integrated system (SOG, System on Glass).
Main purpose of the present invention provides a kind of base plate glass of high strain-point, and this glass has and is fit to be used for generating in its surface the character of polysilicon.
Summary of the invention
The object of the present invention is to provide a kind of have high strain-point, low-expansion coefficient, high elastic coefficient, alkali-free metal oxide, oxygen-free boron, alumina silicate glass that the glass smelting temperature is low and application thereof.
The present invention with following oxide compound by mass percentage (wt.%) be prepared from: SiO
255-70, Al
2O
315-25, CaO 2-11, SrO 1-6, ZnO 3-10, ZrO
21-7, wherein preferred SiO
2+ Al
2O
3Be 79-85, wherein, preferred Al
2O
3Content is 15-25, preferred Al
2O
3Content is 16-22, and preferred CaO content is 4-11, and preferred SrO content is 2-5, and preferred ZnO content is 4-9, preferred ZrO
2Content is 3-6.The density of described glass is less than 2.75g/cm
3, preferably be not more than 2.70g/cm
3Mean coefficient of linear thermal expansion in 30-380 ℃ of scope is (28-38) * 10
-7/ ℃, preferably less than 38 * 10
-7/ ℃; Strain point is preferably greater than 730 ℃ greater than 670 ℃; Young's modulus is preferably greater than 80GPa greater than 75GPa; At room temperature use the NH of 10% concentration
4F-HF buffered soln was handled 20 minutes, and its weight loss is less than 1mg/cm
2, this glass is suitable for making glass integrated system (SOG, System on Glass) and uses base plate glass.
Glass among the present invention is formed, use the overflow down draw explained hereafter, under normal circumstances be not need to carry out milled processed, but,, or take place when using the dull and stereotyped thin glass of overflow down draw explained hereafter when unusual if use production technique such as float glass process, slot draw method, under situations such as glass surface generation scuffing, in order to ensure glass quality, guarantee the yield of product, just need carry out attrition process and handle glass surface.Glass among the present invention is formed, and also can use floating process production.
According to flat-panel monitor, particularly the TFT-LCD display panel is to the character requirement of used base plate glass, preferred glass types is the alkali-free alumina silicate glass that contains alkaline earth metal oxide, such glass has high strain-point, high elastic coefficient, low-expansion characteristics, and has good thermotolerance, chemical-resistant stability etc.
Among the present invention, SiO
2Being the main body that glass forms skeleton, is the composition that plays a major role in the glass skeleton.SiO
2Mass percent (wt.%) be 55-70, SiO
2Content is lower than 55wt.%, is difficult for obtaining the glass of low bulk, high strain-point, can reduce the chemical-resistant stability of glass; SiO
2When content was higher than 70wt.%, the high-temperature viscosity of glass can increase, and caused the glass melting temperature of glass too high.
Al
2O
3The intermediate oxide that belongs to glass, Al
3+Two kinds of co-ordination states are arranged, promptly be arranged in tetrahedron or octahedron, when oxygen is abundant in the glass, form aluminum-oxygen tetrahedron [AlO
4], form the successive network with silicon-oxy tetrahedron, when in the glass during hypoxgia, form alumina octahedral [AlO
6], be in for network outer body in the hole of silica structural network, thus in certain content range can and SiO
2It is the main body that glass network forms.Al
2O
3Mass percent (wt.%) be 15-25.Al
2O
3Content is lower than 15wt.%, is difficult for obtaining high strain-point glass, the chemical-resistant stability deficiency of glass, and the crystallization that can increase glass simultaneously is inclined to; Al
2O
3Content can significantly increase the glass high-temperature viscosity greater than 25wt.%, and the glass melting temperature of glass is raise.
CaO is the glass structure network modifying oxide, and the weight percent of CaO (wt.%) is 2-11, and the content of CaO can reduce the glass chemical-resistant stability greater than 11wt.%, increases the tendency towards devitrification of glass.
SrO is the glass structure network modifying oxide, and the weight percent of SrO (wt.%) is 1-6, and the effect that the content of SrO can increase glass chemistry stability during greater than 6wt.% and improve the anti-devitrification of glass increases the viscosity of founding of glass simultaneously.
ZnO is the glass structure network modifying oxide, and the weight percent of ZnO (wt.%) is 3-10, and the content of ZnO can increase the tendency towards devitrification of glass during greater than 10wt.%.
ZrO
2Be the glass structure network modifying oxide, ZrO
2Weight percent (wt.%) be 1-7, ZrO
2Content can increase the tendency towards devitrification of glass during greater than 7wt.%.
SiO among the present invention
2+ Al
2O
3Total amount at 79-85wt.%, be lower than the glass that 79wt.% then is unfavorable for obtaining low bulk, high strain-point glass, high elastic coefficient, the chemical-resistant stability deficiency of glass, then the glass melting temperature of glass is too high to surpass 85wt.%, liquidus temperature increases, and does not utilize shaping.ZrO
2Weight percent (wt.%) be 1-7, ZrO
2Content can increase the tendency towards devitrification of glass during greater than 7wt.%.
Glass of the present invention belongs to non-alkali glass, alkalimetal oxide R in the glass
2The O total content is less than 0.2wt.% (R=Li, Na, K).Wherein Li, Na, K are not artificial the interpolations, but impurity composition that other frit is brought into.
Glass of the present invention does not also contain environmentally harmful element, as heavy metal element BaO etc.
Embodiment
In table 1, list the glass chemistry of embodiment in detail and formed (wt.%) and glass properties.
(1) density p [g/cm
3];
(2) 30-380 ℃ mean thermal expansion coefficients α
30/380[10
-7/ ℃];
(3) strain point T
St[℃], viscosity is 10
14.5Temperature during dPas;
(4) annealing point T
a[℃], viscosity is 10
13Temperature during dPas;
(5) working point T
w[℃], viscosity is 10
4Temperature during dPas;
(6) Young's modulus (also claiming Young's modulus) E[GPa];
(7) hydrofluoric acid resistant damping fluid corrodibility BHF[mg/cm
2], the glass wafer of polishing both surfaces (diameter Ф=2.5mm, thickness d=2mm) at 25 ℃, with the NH of 10% concentration
4F-HF buffered soln is handled 20 minutes weight loss.
Wherein, the density p of glass adopts Archimedes's drainage to measure; 30-380 ℃ linear expansivity adopts the horizontal expander instrument to measure, and represents with average coefficient of linear expansion, adopts the method for ISO 7991 regulations to measure; The strain point of glass and annealing point adopt the camber beam method of ASTM C598 defined to measure; The Young's modulus of glass adopts the method for ASTM C623 defined to measure; The high-temperature viscosity of glass adopts rotation cartridge type viscosmeter to press ASTM C965-96 method and measures, and calculates working point T by Fulcher formula (being also referred to as the VFT formula)
w
The chemical constitution of table 1 embodiment (wt.%) and glass properties
Embodiment 1
At first, press table 1 embodiment 1 glass composition and select raw material, ingredient requirement, (150 μ m screen overflows are below 1% quartz sand, 45 μ m screen underflows are below 30%, Fe
2O
3Content is less than 0.01wt%), aluminium hydroxide or aluminum oxide (median size 50 μ m), lime carbonate (median size 250 μ m), strontium nitrate or Strontium carbonate powder (median size 50 μ m), zinc oxide (median size 60 μ m screen overflows are below 1%), zirconium silicate or zirconium dioxide (median size 45 μ m screen overflows are below 1%), the alkali metal oxide content in the raw material is less than 0.1%.And Fe in the frit
2O
3Carry out strictness control, finished glass Fe
2O
3Content is less than 150PPm.Finings is a stannic oxide, and the glass chemistry that makes its batching satisfy table 1 is formed, and uses platinum crucible fusion 24 hours under 1570 ℃ of temperature then.After fusion, melten glass liquid is cast into the test article requirement of regulation, anneal then.Its test performance is as shown in table 1, and (1) density is 2.67g/cm
3(2) 30-380 ℃ average coefficient of linear expansion 32.8 * 10
-7/ ℃; (3) strain point T
StIt is 768 ℃; (4) annealing point Ta is 803 ℃; (5) working point T
wIt is 1320 ℃; (6) Young's modulus is 85GPa; (7) hydrofluoric acid resistant damping fluid corrodibility 0.28mg/cm
2
Embodiment 2
The actual composition of glass is with reference to table 1 embodiment 2, uses raw material and the ingredient requirement identical with embodiment 1, and takes identical melting process system and test condition, shown the fundamental property of sample at table 1.(1) density is 2.68g/cm
3(2) 30-380 ℃ average coefficient of linear expansion 32.4 * 10
-7/ ℃; (3) strain point T
StIt is 750 ℃; (4) annealing point T
aIt is 800 ℃; (5) working point T
wIt is 1350 ℃; (6) Young's modulus is 89GPa; (7) hydrofluoric acid resistant damping fluid corrodibility 0.33mg/cm
2
Embodiment 3
The actual composition of glass is with reference to table 1 embodiment 3, uses raw material and the ingredient requirement identical with embodiment 1, and takes identical melting process system and test condition, shown the fundamental property of sample at table 1.(1) density is 2.66g/cm
3(2) 30-380 ℃ average coefficient of linear expansion 31.3 * 10
-7/ ℃; (3) strain point T
StIt is 758 ℃; (4) annealing point T
aIt is 804 ℃; (5) working point T
wIt is 1340 ℃; (6) Young's modulus is 88GPa; (7) hydrofluoric acid resistant damping fluid corrodibility 0.31mg/cm
2
Embodiment 4
The actual composition of glass is with reference to table 1 embodiment 4, uses raw material and the ingredient requirement identical with embodiment 1, and takes identical melting process system and test condition, shown the fundamental property of sample at table 1.(1) density is 2.67g/cm
3(2) 30-380 ℃ average coefficient of linear expansion 31.8 * 10
-7/ ℃; (3) strain point T
StIt is 760 ℃; (4) annealing point T
aIt is 809 ℃; (5) working point T
wIt is 1330 ℃; (6) Young's modulus is 86GPa; (7) hydrofluoric acid resistant damping fluid corrodibility 0.29mg/cm
2
Embodiment 5
The actual composition of glass is with reference to table 1 embodiment 5, uses raw material and the ingredient requirement identical with embodiment 1, and takes identical melting process system and test condition, shown the fundamental property of sample at table 1.(1) density is 2.64g/cm
3(2) 30-380 ℃ average coefficient of linear expansion 32.2 * 10
-7/ ℃; (3) strain point T
StIt is 763 ℃; (4) annealing point T
aIt is 802 ℃; (5) working point T
wIt is 1337 ℃; (6) Young's modulus is 87GPa; (7) hydrofluoric acid resistant damping fluid corrodibility 0.32mg/cm
2
Claims (1)
1. alkali-free alumina silicate glass with high strain point, it is characterized in that: be made of following oxide compound, mass percent is:
SiO
2 55-70
Al
2O
3 15-25
CaO 2-11
SrO 1-6
ZnO 3-10
ZrO
2 1-7。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010237514 CN101913764A (en) | 2010-07-23 | 2010-07-23 | Alkali-free alumina silicate glass with high strain point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010237514 CN101913764A (en) | 2010-07-23 | 2010-07-23 | Alkali-free alumina silicate glass with high strain point |
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| Publication Number | Publication Date |
|---|---|
| CN101913764A true CN101913764A (en) | 2010-12-15 |
Family
ID=43321446
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010237514 Pending CN101913764A (en) | 2010-07-23 | 2010-07-23 | Alkali-free alumina silicate glass with high strain point |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105314846A (en) * | 2014-05-27 | 2016-02-10 | 旭硝子株式会社 | Method for producing alkali-free glass |
| CN112174521A (en) * | 2020-10-30 | 2021-01-05 | 中南大学 | Alkali-free boroaluminosilicate glass for TFT-LCD substrate and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515513A (en) * | 2003-01-02 | 2004-07-28 | 中晶光电科技股份有限公司 | Composition of base plate glass for display |
| CN1640837A (en) * | 2004-01-08 | 2005-07-20 | 郭柏驿 | Base plate glass composition for display device |
| JP2009173525A (en) * | 2007-12-25 | 2009-08-06 | Nippon Electric Glass Co Ltd | Process and apparatus for producing glass plate |
| JP2010064921A (en) * | 2008-09-10 | 2010-03-25 | Ohara Inc | Glass |
-
2010
- 2010-07-23 CN CN 201010237514 patent/CN101913764A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1515513A (en) * | 2003-01-02 | 2004-07-28 | 中晶光电科技股份有限公司 | Composition of base plate glass for display |
| CN1640837A (en) * | 2004-01-08 | 2005-07-20 | 郭柏驿 | Base plate glass composition for display device |
| JP2009173525A (en) * | 2007-12-25 | 2009-08-06 | Nippon Electric Glass Co Ltd | Process and apparatus for producing glass plate |
| JP2010064921A (en) * | 2008-09-10 | 2010-03-25 | Ohara Inc | Glass |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105314846A (en) * | 2014-05-27 | 2016-02-10 | 旭硝子株式会社 | Method for producing alkali-free glass |
| CN105314846B (en) * | 2014-05-27 | 2018-04-24 | 旭硝子株式会社 | Alkali-free glass and its manufacture method |
| CN112174521A (en) * | 2020-10-30 | 2021-01-05 | 中南大学 | Alkali-free boroaluminosilicate glass for TFT-LCD substrate and preparation method thereof |
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Owner name: DONGXU GROUP CO., LTD. Free format text: FORMER OWNER: BEIJING INDUSTRY UNIVERSITY Effective date: 20120426 |
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Effective date of registration: 20120426 Address after: 050021 No. 18, Huitong Road, Hebei, Shijiazhuang Applicant after: Tungsu Group Co., Ltd. Address before: 100124 Chaoyang District, Beijing Ping Park, No. 100 Applicant before: Beijing University of Technology |
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Application publication date: 20101215 |