CN102503141A - Glass-ceramics and preparation method thereof - Google Patents
Glass-ceramics and preparation method thereof Download PDFInfo
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- CN102503141A CN102503141A CN2011103058886A CN201110305888A CN102503141A CN 102503141 A CN102503141 A CN 102503141A CN 2011103058886 A CN2011103058886 A CN 2011103058886A CN 201110305888 A CN201110305888 A CN 201110305888A CN 102503141 A CN102503141 A CN 102503141A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002241 glass-ceramic Substances 0.000 title abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 22
- 239000005357 flat glass Substances 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 20
- 239000013081 microcrystal Substances 0.000 claims description 16
- 229910000500 β-quartz Inorganic materials 0.000 claims description 11
- 238000004090 dissolution Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000006124 Pilkington process Methods 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000007669 thermal treatment Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-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
- 229910000272 alkali metal oxide Inorganic materials 0.000 abstract 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 abstract 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-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
- 238000000465 moulding Methods 0.000 abstract 1
- NOTVAPJNGZMVSD-UHFFFAOYSA-N potassium monoxide Inorganic materials [K]O[K] NOTVAPJNGZMVSD-UHFFFAOYSA-N 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
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 230000035939 shock Effects 0.000 description 8
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 239000000155 melt Substances 0.000 description 4
- 239000002196 Pyroceram Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000006132 parent glass Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 229910000174 eucryptite Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
The invention discloses glass-ceramics and a preparation method of the glass-ceramics. The chemical constitution of the glass-ceramics is formed by the following raw materials selected from one or more of: 50-70 wt% of SiO2, 15-30 wt% of Al2O3, 2-10 wt% of Li2O, 0-9 wt% of B2O3, 0-5 wt% of R2O, 0-10 wt% of RO, 0-5 wt% of TiO2, 0-5 wt% of ZrO2, 0-9 wt% of P2O5 and 0-3 wt% of F, wherein the R2O is one or more of the Li2O, Na2O and K2O; RO is one or more of MgO, CaO, SrO, BaO and ZnO. The glass-ceramics accordance with the requirements can be obtained by the steps of preparing the raw materials, fusing the raw materials, molding glass and carrying out heat treatment. The glass-ceramics and the preparation method of the glass-ceramics, provided by the invention, have the advantages of simple process route, high yield, good product performance, short consumed time and low cost.
Description
Technical field
The present invention relates to a kind of sytull and preparing technical field thereof, specifically a kind of reflection cup, pyroceram panel, the computer hard disk substrate on the projector, sytull of measurement standard spare and preparation method thereof of can be used for.
Background technology
Sytull is Chemical Composition and the exigent specific composition glass of fusing, and becoming after the thermal treatment at a certain temperature has microcrystal and the equally distributed matrix material of glassy phase, is also referred to as glass-ceramic.It has low-expansion coefficient, physical strength height, chemicalstability and premium propertiess such as Heat stability is good, use temperature height and hard wear resistant.Because glass is formed adjustment in very large range, the crystalline phase of separating out is tiny and be evenly distributed because microcrystal glass material have many other materials can't substituted high-performance.Compare with silica glass, sytull has better resistance to air loss owing to having separated out the tiny and uniform crystallite, and therefore obtains higher physical strength; Simultaneously; The coefficient of expansion of sytull can in very large range be regulated through the composition of control crystalline phase; The acquisition of ultra-low-expansion glass ceramic is to separate out crystalline phases such as beta-eucryptite that the C direction of principal axis is negative expansion, β-quartz solid solution, α-eucrytite through the glass kind; And have positive expansible and participate in the glassy phase combination and obtain material near zero thermal expansion even negative expansion; Sytull is in heat treatment process, to control the polycrystalline immobilization material that crystallization obtains the residual glass phase through glass; The crystallite crystalline phase of separating out in the glass is little and be evenly distributed, and making that microcrystal glass material has many other materials can't substituted high-performance, thereby obtains to use widely as structured material, technologic material, electrically insulating material, optical material etc. in fields such as national defence, aviation, transportation, building, production scientific research and lives.
The performance of sytull is to be determined by the chemical constitution of crystalline mineral composition and glassy phase and their quantity, adjusts above-mentioned various factors, just can produce the microcrystal glass material of various pre-determined characteristicss.Mostly the material that is applied in the reflection cup employing on the projector at present is high-boron-silicon glass, and along with the superpower output of projector, volume reduces, and existing high-boron-silicon glass material can not satisfy heat-resisting requirement.Adopt sytull then can effectively improve the heat-resistant quality of reflection cup, the intensity of raising reflection cup satisfies the demand in market.At present the infusibility component is many in the composition of existing sytull, and melt temperature is high, and generally at 1550 ℃ more than-1650 ℃, and the sytull of producing can not satisfy the increasingly high heat shock resistance temperature requirements of reflection cup; Therefore need a kind of sytull that satisfies the reflection cup user demand on the projector of exploitation badly.
Summary of the invention
The objective of the invention is defective, low liquid-crystalline glasses of a kind of heat shock resistance temperature height and melt temperature and preparation method thereof is provided to the prior art existence.
The objective of the invention is to solve through following technical scheme:
A kind of sytull comprises the SiO of following composition: 50-70wt%
2The Al of 15-30wt%
2O
3The Li of 2-10wt%
2O; The B of 0-9wt%
2O
3The R of 0-5wt%
2O, wherein R
2O is Li
2O, Na
2O, K
2Among the O one or more; The RO of 0-10wt%, wherein RO is one or more among MgO, CaO, SrO, BaO, the ZnO.
The TiO that also comprises 0-5wt%
2, 0-5wt% ZrO
2, 0-9wt% P
2O
5With among the F of 0-3wt% one or more.
The composition of the β-quartz solid solution that contains in the described sytull is Li
2O-Al
2O
3-2SiO
2
A kind of preparation method of sytull, described preparation method may further comprise the steps:
(a), feedstock production: according to the chemical constitution of sytull, the weight of weighing desired raw material is put into whisking appliance then and is fully mixed the back as the solid glass raw material in proportion;
(b), raw materials melt: the solid glass raw material for preparing is dropped in the melting furnace; Heating makes the temperature in the melting furnace surpass 1400 ℃ and keep more than the 24h; Can be high temp glass stoste with the solid glass material dissolution, bubble that produces when removing the solid glass material dissolution simultaneously and foreign matter;
(c), glass ware forming: the high temp glass stoste that fusion is good is processed original sheet glass through float glass process or die mould method;
(d), thermal treatment: original sheet glass put in the High Temperature Furnaces Heating Apparatus heat-treat, can in original sheet glass, generate the low bulk β-quartz solid solution crystallite of homogeneous after thermal treatment finishes, obtain satisfactory sytull.
Heat treatment process in the said step (d) comprises that microcrystals is separated out and crystallite is grown up two stages.
The required temperature of microcrystals precipitation phase in said step (d) heat treatment process is 550 ℃-650 ℃, and the time length is 1-3h.
Required temperature of the crystallite stage of growth in said step (d) heat treatment process is 700 ℃-800 ℃, and the time length is 1-2h.
The whisking appliance that adopts in the said step (a) is the V-type whisking appliance.
The melting furnace that adopts in the said step (b) is electric furnace or crucible oven.
The present invention compares prior art has following advantage:
Sytull heat shock resistance temperature of the present invention can reach about 700 ℃, has promoted the heat shock resistance temperature of sytull greatly, and has passed through TiO
2, ZrO
2, P
2O
5, F adding, make this sytull microcrystals separate out more even; And the adding through MOX, the melt temperature of sytull raw material has been reduced to 1400 ℃-1500 ℃, greatly reduce the melt temperature of sytull, saved production cost.
Operational path of the present invention sytull heat shock resistance temperature simple, that produce is high, physical strength is high, has satisfied the user demand of the reflection cup on the projector, pyroceram panel, computer hard disk substrate, measurement standard spare; And have yield rate height, good product performance, weak point consuming time and low characteristics of cost.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
Embodiment 1
At first according to weight ratio with 58% SiO
2, 21% Al
2O
3, 6% Li
2O, 4% B
2O
3, 2% Na
2O and K
2The mixture of the mixture of O, 5% MgO and CaO and 1.5% TiO
2, 1% ZrO
2, 2.5% P
2O
5Come out with 1% F weighing, then it is all put into the V-type whisking appliance and fully mix the back as the solid glass raw material; Then the solid glass raw material for preparing is dropped in electric furnace or the crucible oven; Heating makes the temperature in the stove surpass 1400 ℃ and keep more than the 24h; Can be high temp glass stoste with the solid glass material dissolution, bubble that produces when removing the solid glass material dissolution simultaneously and foreign matter; Then that fusion is good high temp glass stoste is processed original sheet glass through float glass process or die mould method; At last the original sheet glass that makes being put into High Temperature Furnaces Heating Apparatus heat-treats; This heat treatment process comprises that microcrystals is separated out and crystallite is grown up two stages; Wherein in the microcrystals precipitation phase; Temperature in the High Temperature Furnaces Heating Apparatus is remained on about 590 ℃, and lasting 2.5h makes and produce polycrystallite nuclear as far as possible in the original sheet glass, then the temperature in the High Temperature Furnaces Heating Apparatus is elevated to and enters into the crystallite stage of growth about 730 ℃ and continue 1.5h; Can in original sheet glass, generate the low bulk β-quartz solid solution crystallite of homogeneous; Obtain satisfactory sytull, then will be converted into the microlitic structure by parent glass at this stage original sheet glass is main sytull, and its composition that contains β-quartz solid solution is Li
2O-Al
2O
3-2SiO
2
Embodiment 2
At first according to weight ratio with 63% SiO
2, 18% Al
2O
3, 6% Li
2O, 2% B
2O
3, 3% Na
2O and K
2The mixture of the mixture of O, 4% CaO, SrO and BaO and 0.8% TiO
2, 1.2% ZrO
2, 1.5% P
2O
5Come out with 0.5% F weighing, then it is all put into the V-type whisking appliance and fully mix the back as the solid glass raw material; Then the solid glass raw material for preparing is dropped in electric furnace or the crucible oven; Heating makes the temperature in the stove surpass 1420 ℃ and keep more than the 24h; Can be high temp glass stoste with the solid glass material dissolution, bubble that produces when removing the solid glass material dissolution simultaneously and foreign matter; Then that fusion is good high temp glass stoste is processed original sheet glass through float glass process or die mould method; At last the original sheet glass that makes being put into High Temperature Furnaces Heating Apparatus heat-treats; This heat treatment process comprises that microcrystals is separated out and crystallite is grown up two stages; Wherein in the microcrystals precipitation phase; Temperature in the High Temperature Furnaces Heating Apparatus is remained on about 640 ℃, and lasting 2h makes and produce polycrystallite nuclear as far as possible in the original sheet glass, then the temperature in the High Temperature Furnaces Heating Apparatus is elevated to and enters into the crystallite stage of growth about 780 ℃ and continue 1.2h; Can in original sheet glass, generate the low bulk β-quartz solid solution crystallite of homogeneous; Obtain satisfactory sytull, then will be converted into the microlitic structure by parent glass at this stage original sheet glass is main sytull, and its composition that contains β-quartz solid solution is Li
2O-Al
2O
3-2SiO
2
Embodiment 3
At first according to weight ratio with 52% SiO
2, 20% Al
2O
3, 8% Li
2O, 6% B
2O
3, 1.5% Na
2O and K
2The mixture of the mixture of O, 5.5% MgO, SrO and ZnO and 2% TiO
2, 2.5% ZrO
2, 1.5% P
2O
5Come out with 1% F weighing, then it is all put into the V-type whisking appliance and fully mix the back as the solid glass raw material; Then the solid glass raw material for preparing is dropped in electric furnace or the crucible oven; Heating makes the temperature in the stove surpass 1450 ℃ and keep more than the 24h; Can be high temp glass stoste with the solid glass material dissolution, bubble that produces when removing the solid glass material dissolution simultaneously and foreign matter; Then that fusion is good high temp glass stoste is processed original sheet glass through float glass process or die mould method; At last the original sheet glass that makes being put into High Temperature Furnaces Heating Apparatus heat-treats; This heat treatment process comprises that microcrystals is separated out and crystallite is grown up two stages; Wherein in the microcrystals precipitation phase; Temperature in the High Temperature Furnaces Heating Apparatus is remained on about 600 ℃, and lasting 2h makes and produce polycrystallite nuclear as far as possible in the original sheet glass, then the temperature in the High Temperature Furnaces Heating Apparatus is elevated to and enters into the crystallite stage of growth about 750 ℃ and continue 1.6h; Can in original sheet glass, generate the low bulk β-quartz solid solution crystallite of homogeneous; Obtain satisfactory sytull, then will be converted into the microlitic structure by parent glass at this stage original sheet glass is main sytull, and its composition that contains β-quartz solid solution is Li
2O-Al
2O
3-2SiO
2
Sytull heat shock resistance temperature of the present invention can reach about 700 ℃, has promoted the heat shock resistance temperature of sytull greatly, and has passed through TiO
2, ZrO
2, P
2O
5, F adding, make this sytull microcrystals separate out more even; And through MOX and vitrifying composition B
2O
3Adding, the melt temperature of sytull raw material has been reduced to 1400 ℃-1500 ℃, greatly reduce the melt temperature of sytull, saved production cost.Operational path of the present invention in addition sytull heat shock resistance temperature simple, that produce is high, physical strength is high, has satisfied the user demand of the reflection cup on the projector, pyroceram panel, computer hard disk substrate, measurement standard spare; And have yield rate height, good product performance, weak point consuming time and low characteristics of cost.
The present invention does not relate to all identical with the prior art prior art that maybe can adopt of part and realizes.
Claims (9)
1. a sytull is characterized in that, comprises the SiO of following composition: 50-70wt%
2The Al of 15-30wt%
2O
3The Li of 2-10wt%
2O; The B of 0-9wt%
2O
3The R of 0-5wt%
2O, wherein R
2O is Li
2O, Na
2O, K
2Among the O one or more; The RO of 0-10wt%, wherein RO is one or more among MgO, CaO, SrO, BaO, the ZnO.
2. sytull according to claim 1 is characterized in that, also comprises the TiO of 0-5wt%
2, 0-5wt% ZrO
2, 0-9wt% P
2O
5With among the F of 0-3wt% one or more.
3. sytull according to claim 2, the composition of the β-quartz solid solution that it is characterized in that containing in the described sytull is Li
2O-Al
2O
3-2SiO
2
4. the preparation method of a sytull is characterized in that described preparation method may further comprise the steps:
(a), feedstock production: according to the chemical constitution of sytull, the weight of weighing desired raw material is put into whisking appliance then and is fully mixed the back as the solid glass raw material in proportion;
(b), raw materials melt: the solid glass raw material for preparing is dropped in the melting furnace; Heating makes the temperature in the melting furnace surpass 1400 ℃ and keep more than the 24h; Can be high temp glass stoste with the solid glass material dissolution, bubble that produces when removing the solid glass material dissolution simultaneously and foreign matter;
(c), glass ware forming: the high temp glass stoste that fusion is good is processed original sheet glass through float glass process or die mould method;
(d), thermal treatment: original sheet glass put in the High Temperature Furnaces Heating Apparatus heat-treat, can in original sheet glass, generate the low bulk β-quartz solid solution crystallite of homogeneous after thermal treatment finishes, obtain satisfactory sytull.
5. the preparation method of sytull according to claim 4 is characterized in that the heat treatment process in the said step (d) comprises that microcrystals is separated out and crystallite is grown up two stages.
6. the preparation method of sytull according to claim 5 is characterized in that the required temperature of microcrystals precipitation phase in said step (d) heat treatment process is 550 ℃-650 ℃, and the time length is 1-3h.
7. the preparation method of sytull according to claim 5 is characterized in that the required temperature of the crystallite stage of growth in said step (d) heat treatment process is 700 ℃-800 ℃, and the time length is 1-2h.
8. the preparation method of sytull according to claim 4 is characterized in that the whisking appliance that adopts in the said step (a) is the V-type whisking appliance.
9. the preparation method of sytull according to claim 4 is characterized in that the melting furnace that adopts in the said step (b) is electric furnace or crucible oven.
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110305888.6A CN102503141B (en) | 2011-10-11 | 2011-10-11 | Glass-ceramics and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN102503141A true CN102503141A (en) | 2012-06-20 |
| CN102503141B CN102503141B (en) | 2014-02-26 |
Family
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104370469A (en) * | 2014-10-28 | 2015-02-25 | 蒋达光 | Colorful glass ceramic with ultralow expansion coefficient and high transparency, and parathion method thereof |
| CN104743884A (en) * | 2015-03-25 | 2015-07-01 | 河北省沙河玻璃技术研究院 | Glass ceramic and float producing process thereof |
| CN104876447A (en) * | 2015-05-14 | 2015-09-02 | 西安交通大学 | Preparation method of Li-Al-Si porous microcrystalline glass |
| CN105731809A (en) * | 2014-12-11 | 2016-07-06 | 北京有色金属研究总院 | Insulating material for heating wire, preparation and application method thereof |
| CN107117821A (en) * | 2017-06-30 | 2017-09-01 | 合肥利裕泰玻璃制品有限公司 | A kind of high strength micro-crystalline glass and preparation method thereof |
| CN107974763A (en) * | 2017-11-17 | 2018-05-01 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of low melting point crystalline glass fibre cotton and preparation method thereof |
| CN108218237A (en) * | 2018-01-29 | 2018-06-29 | 南通向阳光学元件有限公司 | A kind of preparation method of devitrified glass |
| CN111094202A (en) * | 2017-08-31 | 2020-05-01 | 康宁股份有限公司 | Yaoshi karite glass-ceramics obtained from glass frit |
| CN112456806A (en) * | 2018-10-26 | 2021-03-09 | 成都光明光电股份有限公司 | Glass ceramics, glass ceramics product and manufacturing method thereof |
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| CN116553833A (en) * | 2023-03-23 | 2023-08-08 | 成都光明光电有限责任公司 | Low-expansion glass ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104370469A (en) * | 2014-10-28 | 2015-02-25 | 蒋达光 | Colorful glass ceramic with ultralow expansion coefficient and high transparency, and parathion method thereof |
| CN105731809A (en) * | 2014-12-11 | 2016-07-06 | 北京有色金属研究总院 | Insulating material for heating wire, preparation and application method thereof |
| CN104743884A (en) * | 2015-03-25 | 2015-07-01 | 河北省沙河玻璃技术研究院 | Glass ceramic and float producing process thereof |
| CN104876447A (en) * | 2015-05-14 | 2015-09-02 | 西安交通大学 | Preparation method of Li-Al-Si porous microcrystalline glass |
| CN107117821A (en) * | 2017-06-30 | 2017-09-01 | 合肥利裕泰玻璃制品有限公司 | A kind of high strength micro-crystalline glass and preparation method thereof |
| CN111094202A (en) * | 2017-08-31 | 2020-05-01 | 康宁股份有限公司 | Yaoshi karite glass-ceramics obtained from glass frit |
| CN107974763A (en) * | 2017-11-17 | 2018-05-01 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of low melting point crystalline glass fibre cotton and preparation method thereof |
| CN108218237A (en) * | 2018-01-29 | 2018-06-29 | 南通向阳光学元件有限公司 | A kind of preparation method of devitrified glass |
| CN112456806A (en) * | 2018-10-26 | 2021-03-09 | 成都光明光电股份有限公司 | Glass ceramics, glass ceramics product and manufacturing method thereof |
| 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 |
| CN116553833A (en) * | 2023-03-23 | 2023-08-08 | 成都光明光电有限责任公司 | Low-expansion glass ceramic and preparation method thereof |
| CN117756411A (en) * | 2023-12-21 | 2024-03-26 | 清远南玻节能新材料有限公司 | Microcrystalline glass and preparation method thereof |
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