CN1847182A - Ultralow thermal expansion devitrified glass - Google Patents
Ultralow thermal expansion devitrified glass Download PDFInfo
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- CN1847182A CN1847182A CNA2005100250953A CN200510025095A CN1847182A CN 1847182 A CN1847182 A CN 1847182A CN A2005100250953 A CNA2005100250953 A CN A2005100250953A CN 200510025095 A CN200510025095 A CN 200510025095A CN 1847182 A CN1847182 A CN 1847182A
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- China
- Prior art keywords
- crystallization
- coring
- thermal expansion
- ultra
- devitrified glass
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- 239000011521 glass Substances 0.000 title claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims description 13
- 230000008025 crystallization Effects 0.000 claims description 13
- 239000002241 glass-ceramic Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000010079 rubber tapping Methods 0.000 abstract description 2
- GOLCXWYRSKYTSP-UHFFFAOYSA-N Arsenious Acid Chemical compound O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- 238000003723 Smelting Methods 0.000 abstract 1
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 abstract 1
- 238000007689 inspection Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 5
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- JRIGVWDKYXCHMG-UHFFFAOYSA-N (5-arsoroso-2-hydroxyphenyl)azanium;chloride Chemical compound Cl.NC1=CC([As]=O)=CC=C1O JRIGVWDKYXCHMG-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000012952 Resampling Methods 0.000 description 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N Vanadium(V) oxide Inorganic materials O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical class [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 229910000413 arsenic oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229950008475 oxophenarsine Drugs 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
-
- 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The present invention discloses one kind of ultralow thermal expansion devitrified glass used for reflector, planar mirror, template and other precise optical elements. It has the material composition of: SiO2 47.2-49.1(in wt%, the same as below),Al2O3 27.6-29.0,Sb2O3 0.78-0.82,As2O3 0.30-0.35,BaO 2.98-3.05,ZnO 2.00-2.05, CaO 2.28-2.33,MgO 0.5-1.0,Li2O 7.1-7.5,P2O5 4.0-4.4,ZrO2 1.2-1.7 and TiO2 1.4-1.5 . The technological process includes the following steps: mixing the components, high temperature smelting in high temperature quartz-ceramic crucible at 1580-1630 deg.c, tapping at 1450 deg.c, forming, inspection, nucleating at 660-690 deg.c, crystallizing at 690-720 deg.c, precise annealing at 640-540 deg.c.
Description
Affiliated technical field
The present invention is a trade mark in the big class of lithium aluminium silicon series devitrified glass, is the material that is used for large-scale astronomical telescope mirror embryo, precision optics speculum, flat mirror, model, quarter chi, grating substrate, processing template, laser gyro cavity.
Background technology
At present, the devitrified glass coefficient of expansion that is used for the speculum of precision optics, flat mirror, model, quarter chi, grating substrate, processing template, laser gyro cavity is difficult to meet the demands than higher.
Summary of the invention
The object of the present invention is to provide a kind of coefficient of expansion (α), melting performance, the well behaved a kind of ultra-low-expansion glass ceramic of crystallization.
The present invention is selecting SiO
2, Al
2O
3, Sb
2O
3, As
2O
3, BaO, ZnO, CaO, MgO, Li
2O, P
2O
5, ZrO
2, TiO
2On the basis of system, SiO in will filling a prescription
2, Al
2O
3, Li
2O, P
2O
5, ZrO
2Adjust Deng oxide compound, adopt high melt, moulding, check, coring, crystallization, performance test processing step to realize its purpose.
Ultra-low-expansion glass ceramic V of the present invention
02, Liang component is SiO by weight percentage
2---47.2-49.1, Al
2O
3---27.6-29.0, Sb
2O
3---0.78-0.82, As
2O
3---0.30-0.35, BaO---2.98-3.05, ZnO---2.00-2.05, CaO---2.28-2.33, MgO---0.5-1.0, Li
2O---7.1-7.5, P
2O
5---4.0-4.4, ZrO
2---1.2-1.7, TiO
2---1.4-1.5, said components is mixed, found through 1580～1630 ℃, come out of the stove for 1450 ℃, moulding, check, again through 660～690 ℃ of coring, through 690～720 ℃ of crystallization, 640～540 ℃ of fine annealings record α :≤0 ± 0.7 * 10 after the cooling
-7/ ℃ (50～60 ℃), stress birefringence≤10nm/cm, bubble, striped index meet the requirements of ultra-low-expansion glass ceramic.
Increase Li in the above-mentioned prescription
2O, ZrO
2Can adjust coring, crystallization performance, MgO, P
2O
5The transparency of improving glass is beneficial to.
Adopt above-mentioned prescription to make ultra-low-expansion glass ceramic V
02The time, at first adopt new proportioning process that each component is mixed, adopt the high melt Technology, in high temperature resistant quartz ceramic crucible, found through 1580～1630 ℃, come out of the stove for 1450 ℃, moulding, check is again through 660～690 ℃ of coring, through 690～720 ℃ of crystallization, 640～540 ℃ of fine annealings.
Embodiment
The present invention is further described with embodiment below.
The component of embodiments of the invention 1～5, processing parameter, performance perameter such as following table are listed:
| Component | Technical parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| SiO 2 | (weight part) | 48.53 | 48.44 | 47.2 | 47.7 | 49.1 |
| Al 2O 3 | (weight part) | 27.8 | 27.89 | 29.0 | 28.84 | 27.6 |
| Sb 2O 3 | (weight part) | 0.81 | 0.82 | 0.78 | 0.80 | 0.80 |
| As 2O 3 | (weight part) | 0.30 | 0.32 | 0.32 | 0.32 | 0.35 |
| BaO | (weight part) | 3.03 | 3.05 | 3.01 | 3.00 | 3.00 |
| ZnO | (weight part) | 2.03 | 2.05 | 2.02 | 2.01 | 2.00 |
| CaO | (weight part) | 2.33 | 2.32 | 2.32 | 2.29 | 2.28 |
| MgO | (weight part) | 0.50 | 0.59 | 0.58 | 0.83 | 1.0 |
| Li 2O | (weight part) | 7.49 | 7.50 | 7.44 | 7.10 | 7.20 |
| P 2O 5 | (weight part) | 4.23 | 4.06 | 4.40 | 4.01 | 4.00 |
| ZrO 2 | (weight part) | 1.46 | 1.46 | 1.45 | 1.70 | 1.20 |
| TiO 2 | (weight part) | 1.49 | 1.50 | 1.48 | 1.40 | 1.47 |
| Add up to | (weight part) | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 |
| Charge temperature (℃) | 1480 | 1480 | 1460 | 1460 | 1500 | |
| Glass melting temperature (℃) | 1620 | 1620 | 1620 | 1620 | 1630 | |
| Tapping temperature (℃) | 1450 | 1450 | 1450 | 1450 | 1450 | |
| Nucleation temperature (℃) | 680 | 680 | 670 | 680 | 690 | |
| Crystallization temperature (℃) | 700 | 700 | 710 | 715 | 720 | |
| Annealing temperature (℃) | 650 | 650 | 650 | 650 | 650 | |
| The coefficient of expansion (* 10 -7/℃) (-50～60℃) | 0.5 | 0.3 | 0.7 | 0.6 | 1.0 |
Adopt above-mentioned prescription to make ultra-low-expansion glass ceramic V
02The time, at first each component is mixed, adopt the high melt Technology, in high temperature resistant quartz ceramic crucible, found through 1580～1630 ℃, come out of the stove for 1450 ℃, moulding, check, again through 660～690 ℃ of coring, through 690～720 ℃ of crystallization, 640～540 ℃ of fine annealings.
The above embodiment of the present invention manufacturing process program is basic identical, just selects recipe ingredient slightly different, and main purpose is in order to adjust coring, crystallization performance and the coefficient of expansion.Above embodiment all founds in 4500ml quartz ceramic crucible molybdenum bar electric furnace, pouring technology is adopted in moulding, coring, crystallization, annealing are carried out in accurate crystallization furnace, annealing process: 650 ℃ are incubated 3 hours, drop to 400 ℃ with 10 ℃/hour, powered-down is cooled to room temperature, the inner quality of sight glass, the resampling product carry out the test of the coefficient of expansion.
Can go into operation 50L electric furnace and 8 tons of pneumoelectrics heating tank furnaces of this trade mark are produced in batches.
The chemical feedstocks explanation:
SiO
2Silicon oxide
Al
2O
3Aluminum oxide
Sb
2O
3Weisspiessglanz
As
2O
3Arsenic oxide arsenoxide
BaO barium oxide
ZnO zinc oxide
The CaO calcium oxide
MgO magnesium oxide
Li
2The O Lithium Oxide 98min
P
2O
5Vanadium Pentoxide in FLAKES
ZrO
2Zirconium white
TiO
2Titanium oxide
Claims (2)
1, a kind of ultra-low-expansion glass ceramic is characterized in that: Liang component is SiO by weight percentage
2-47.2-49.1, Al
2O
3-27.6-29.0, Sb
2O
3-0.78-0.82, As
2O
3-0.30-0.35, BaO-2.98-3.05, ZnO-2.00-2.05, CaO-2.28-2.33, MgO-0.5-1.0, Li
2O-7.1-7.5, P
2O
5-4.0-4.4, ZrO
2-1.2-1.7, TiO
2-1.4-1.5.
2, a kind of production technique of ultra-low-expansion glass ceramic, at first each component is mixed, adopt the high melt Technology, in high temperature resistant quartz ceramic crucible, found through 1580～1630 ℃, come out of the stove for 1450 ℃, moulding, check is again through 660～690 ℃ of coring, through 690～720 ℃ of crystallization, 640～540 ℃ of fine annealings; Pouring technology is adopted in moulding, and annealing process is carried out in coring, crystallization, annealing in accurate crystallization furnace: 650 ℃ of insulations 3 hours, drop to 400 ℃ with 10 ℃/hour, and powered-down is cooled to room temperature and takes out glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2005100250953A CN1847182A (en) | 2005-04-14 | 2005-04-14 | Ultralow thermal expansion devitrified glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2005100250953A CN1847182A (en) | 2005-04-14 | 2005-04-14 | Ultralow thermal expansion devitrified glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1847182A true CN1847182A (en) | 2006-10-18 |
Family
ID=37076959
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2005100250953A Pending CN1847182A (en) | 2005-04-14 | 2005-04-14 | Ultralow thermal expansion devitrified glass |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1847182A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857373A (en) * | 2010-06-03 | 2010-10-13 | 香港福山实业有限公司 | A glass-ceramic tube and its preparation method |
| CN102503102A (en) * | 2011-09-29 | 2012-06-20 | 中国航空工业第六一八研究所 | A super-stabilizing treatment method for ultra-low expansion glass-ceramic |
| CN110217985A (en) * | 2019-07-04 | 2019-09-10 | 广东科迪微晶玻璃实业有限公司 | A kind of production method of low-expansion coefficient transparent glass-ceramics and its product |
| CN111807706A (en) * | 2020-06-29 | 2020-10-23 | 成都光明光电股份有限公司 | Glass ceramics and glass ceramics product |
| CN111943514A (en) * | 2020-06-29 | 2020-11-17 | 成都光明光电股份有限公司 | Glass-ceramic and glass-ceramic article |
-
2005
- 2005-04-14 CN CNA2005100250953A patent/CN1847182A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857373A (en) * | 2010-06-03 | 2010-10-13 | 香港福山实业有限公司 | A glass-ceramic tube and its preparation method |
| CN102503102A (en) * | 2011-09-29 | 2012-06-20 | 中国航空工业第六一八研究所 | A super-stabilizing treatment method for ultra-low expansion glass-ceramic |
| CN102503102B (en) * | 2011-09-29 | 2014-12-24 | 中国航空工业第六一八研究所 | Ultra-low expansion glass ceramic ultra-stabilization treatment method |
| CN110217985A (en) * | 2019-07-04 | 2019-09-10 | 广东科迪微晶玻璃实业有限公司 | A kind of production method of low-expansion coefficient transparent glass-ceramics and its product |
| CN111807706A (en) * | 2020-06-29 | 2020-10-23 | 成都光明光电股份有限公司 | Glass ceramics and glass ceramics product |
| CN111943514A (en) * | 2020-06-29 | 2020-11-17 | 成都光明光电股份有限公司 | Glass-ceramic and glass-ceramic article |
| CN114671619A (en) * | 2020-06-29 | 2022-06-28 | 成都光明光电股份有限公司 | Glass ceramics and glass ceramics product |
| CN114671619B (en) * | 2020-06-29 | 2023-12-05 | 成都光明光电股份有限公司 | Glass ceramics and glass ceramics products |
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Open date: 20061018 |