CN108623166A - A kind of intelligent light-controlled glass high rigidity substrate and preparation method thereof - Google Patents

A kind of intelligent light-controlled glass high rigidity substrate and preparation method thereof Download PDF

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Publication number
CN108623166A
CN108623166A CN201810607454.3A CN201810607454A CN108623166A CN 108623166 A CN108623166 A CN 108623166A CN 201810607454 A CN201810607454 A CN 201810607454A CN 108623166 A CN108623166 A CN 108623166A
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parts
substrate
temperature
high rigidity
oxide
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CN201810607454.3A
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Inventor
秦世明
赵光勇
赵洁
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ZHEJIANG XIXI GLASS CO Ltd
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ZHEJIANG XIXI GLASS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified 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
    • C03C10/0018Devitrified 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 containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention relates to intelligent glass field, a kind of intelligent light-controlled glass high rigidity substrate and preparation method thereof is disclosed.The substrate contains following components and parts by weight:80 120 parts of silica, 10 15 parts of sodium oxide molybdena, 79 parts of calcium oxide, 15 20 parts of aluminium oxide, 35 parts of magnesia, 24 parts of zinc oxide, 1.5 2.5 parts of yttria, 2.8 3.2 parts of zirconium dioxide, 2.5 3.5 parts of antimony oxide, 13 parts of phosphorus pentoxide, 35 parts of titanium dioxide.The preparation method of the present invention is simple for process, and Mohs' hardness >=8,1mm visible light transmittance of gained substrate is more than 80%, has the physical and chemical performance of the transparency height of glass and the high rigidity of ceramics concurrently, overcomes the problem of existing intelligent light-controlled glass is easy to scratch.

Description

A kind of intelligent light-controlled glass high rigidity substrate and preparation method thereof
Technical field
The present invention relates to intelligent glass field more particularly to a kind of intelligent light-controlled glass high rigidity substrate and its preparation sides Method.
Background technology
Intelligent light-controlled glass is that one layer of liquid crystal film is clipped between layer glass, liquid crystal film be covered in by PVB films it is most central, so It is placed on autoclave or general one-step method stove back warp is crossed the process gluing of high temperature and pressure and formed.Intelligent light-controlled glass is in addition to tool Standby privacy protection function, is provided simultaneously with the application characteristic of all safety glasses.Due to intelligent light-controlled glass construction complexity, cost compared with Height is not easy to grind colored damage, reduces transport and service wear therefore it is required that the hardness of glass substrate is higher, reduces cost, and conventional Float glass or ultra-clear glasses this requirement is all not achieved.
Invention content
In order to solve the above technical problem, the present invention provides a kind of intelligent light-controlled glass high rigidity substrate and its preparations Method.By adjusting the component of glass substrate, with when preparation process, obtained being suitable for the high rigidity that intelligent light-controlled glass uses High grade of transparency substrate.
The specific technical solution of the present invention is:The substrate contains following components and parts by weight:80-120 parts of silica, oxygen Change 10-15 parts of sodium, 7-9 parts of calcium oxide, 15-20 parts of aluminium oxide, 3-5 parts of magnesia, 2-4 parts of zinc oxide, yttria 1.5- 2.5 parts, 2.8-3.2 parts of zirconium dioxide, 2.5-3.5 parts of antimony oxide, 1-3 parts of phosphorus pentoxide, 3-5 parts of titanium dioxide.
SiO2It is important glass former oxide, with oxygen-octahedron [SiO4] structural unit formed it is irregular Contiguous network becomes the skeleton of glass.Its content affects the endurance and mechanical strength of glass, in addition also to the density of glass Also it will produce influence.Content is higher, and the chemical resistance and mechanical strength of glass are higher.On the other hand, due to having raising viscosity Tendency, content is too high, increases the high temperature viscosity of glass, and glass is made to be difficult to melt.
Al2O3It is the neccessary composition for improving chemical durability of glass.
MgO、ZnO、Na2O and CaO is the network modifying oxide of glass, can reduce the viscosity of glass, promotes glass Fusing and clarification, improve forming of glass performance, and a certain amount of network modifying oxide can improve the hardness of glass, chemistry Stability, thermal stability and mechanical strength.But Na2O can reduce thermal stability, chemical stability and the mechanical strength of glass.CaO When higher, the tendency of glass can be made to increase, and easily make glass embrittlement.When the content of MgO and ZnO is higher, it can go out in glass Existing other crystal, can reduce the transparency of glass in this way.Therefore when the network modifying oxide introduction volume of glass is less, Ke Yiyu Other oxide collective effects improve the mechanical performance of glass, but when the amount replaced is excessive, and the mechanical performance of glass can be significantly Reduction.
Yttria has stronger accumulation to act on, and can promote the densification of glass structure, in addition, yttria can To play the role of stabilizer, zirconium dioxide is stablized in tetragonal phase, nucleating effect is improved;Phosphorus pentoxide can increase dioxy Change the solubility of zirconium in the melt, while the melt temperature of zirconium dioxide can be reduced;And zirconium dioxide is as Nucleating Agent, it can be with Nucleation and crystallization activation energy are reduced, nucleation rate is accelerated, promotes glass coring and crystallization, the four directions oxidation that yttria is stablized Zirconium effect is more excellent, and can organize excessively growing up for nucleus, reduces out-phase crystallization.Three can reduce into as Composite Nucleation Agents Nuclear barrier promotes nucleation and crystallization, improves the crystallization property of glass, can preferably obtain the glass of crystalline phase single stable, pole Big limits its out-phase crystallization in crystallization process, while can reduce the defects of glass, improve glass hardness and Mechanical performance can meet intelligent light-controlled glass to substrate high rigidity, wear-resisting requirement.
Titanium dioxide can reduce crystallization temperature, promote crystallization.
Alkaline earth oxide has " mixed alkali effect ", refers under conditions of the total content of alkaline earth oxide is constant, Another or two kinds, performance change curve not instead of straight line is replaced to change a kind of alkaline earth oxide, There is extreme value in specific position, therefore the additive amount of alkaline earth oxide is difficult to find rule.
Preferably, the substrate contains following components and parts by weight:00 part of silica 1,12 parts of sodium oxide molybdena, calcium oxide 8 Part, 18 parts of aluminium oxide, 4 parts of magnesia, 3 parts of zinc oxide, 2 parts of yttria, 3 parts of zirconium dioxide, 3 parts of antimony oxide, five Aoxidize 2 parts of two phosphorus, 4 parts of titanium dioxide.
The preparation method of the substrate comprises the steps of:
1)Raw material is chosen, is sufficiently mixed after weighing in proportion, obtains mixture;
2)Mixture is placed in smelting furnace and is warming up to melting, keeps the temperature 1.5-2h, then rapid shaping;
3)Annealing;
4)Coring is handled;
5)Crystallizing treatment;
6)Etch is handled.
It is made annealing treatment, by the heating and heat preservation temperature-fall period of multistep, the toughness and hardness of glass can be effectively improved; After annealing, coring processing and Crystallizing treatment are carried out, high rigidity glass substrate can be finally obtained.
Preferably, the step 2)Middle melting temperature is 1650-1700 DEG C.
Preferably, the step 3)Middle annealing specific method is:Substrate after molding is warming up to 200 DEG C, is protected Warm 1h, air cooling is to room temperature, then is warming up to 250 DEG C, keeps the temperature 1h, and air cooling is to room temperature, then is warming up to 300 DEG C, keeps the temperature 1h, Air cooling then heats to 500 DEG C to room temperature, keeps the temperature 1h.
Preferably, the step 4)Middle coring processing method is:Substrate after annealing is warming up to 850 DEG C, keeps the temperature 3h.
Preferably, the step 5)Middle Crystallizing treatment method is:Substrate after coring is warming up to 1000 DEG C, heat preservation 2h。
Preferably, the step 6)Middle etching handling method is:Substrate surface acid soak is handled into 30min, then Substrate is finally kept the temperature 2h by supersound washing 1h at 1200-1350 DEG C.
Etch processing can enable the glass surface after annealing, coring, crystallization more smooth, and substrate thickness is thinner, light transmission Effect is more preferable.
Preferably, the acid solution is the hydrofluoric acid of 2-2.8wt%.
It is compared with the prior art, the beneficial effects of the invention are as follows:The preparation method of the present invention is simple for process, gained intelligence light Control glass high rigidity substrate Mohs' hardness >=8,1mm visible light transmittance be more than 80%, have concurrently glass transparency height and The physical and chemical performance of the high rigidity of ceramics;The substrate of the present invention has high mechanical strength, high thermal stability, good chemistry steady It is qualitative, wearability is good, preferable visible optical property, overcome the problem of existing intelligent light-controlled glass is easy to scratch.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
Choose raw material:00 part of silica 1,12 parts of sodium oxide molybdena, 8 parts of calcium oxide, 18 parts of aluminium oxide, 4 parts of magnesia, zinc oxide 3 Part, 2 parts of yttria, 3 parts of zirconium dioxide, 3 parts of antimony oxide, 2 parts of phosphorus pentoxide, 4 parts of titanium dioxide.Claim in proportion It is sufficiently mixed after amount, obtains mixture;Mixture is placed in smelting furnace and is warming up to 1700 DEG C, keeps the temperature 1.5h, then rapid shaping; Substrate after molding is warming up to 200 DEG C, keeps the temperature 1h, air cooling is to room temperature, then is warming up to 250 DEG C, keeps the temperature 1h, air cooling To room temperature, then 300 DEG C are warming up to, keep the temperature 1h, air cooling to room temperature then heats to 500 DEG C, keeps the temperature 1h.After annealing Substrate is warming up to 850 DEG C, keeps the temperature 3h.Substrate after coring is warming up to 1000 DEG C, keeps the temperature 2h.Substrate is impregnated to the hydrogen of 2.5wt% Fluoric acid handles 30min, and then substrate, is finally kept the temperature 2h by supersound washing 1h at 1250 DEG C.
Embodiment 2
Choose raw material:80 parts of silica, 15 parts of sodium oxide molybdena, 7 parts of calcium oxide, 20 parts of aluminium oxide, 3 parts of magnesia, zinc oxide 4 Part, 1.5 parts of yttria, 3.2 parts of zirconium dioxide, 2.5 parts of antimony oxide, 1 part of phosphorus pentoxide, 5 parts of titanium dioxide.It presses Ratio is sufficiently mixed after weighing, and obtains mixture;Mixture is placed in smelting furnace and is warming up to 1650 DEG C, keeps the temperature 2h, then quickly Molding;Substrate after molding is warming up to 200 DEG C, keeps the temperature 1h, air cooling is to room temperature, then is warming up to 250 DEG C, keeps the temperature 1h, empty Air cooling is to room temperature, then is warming up to 300 DEG C, keeps the temperature 1h, and air cooling to room temperature then heats to 500 DEG C, keeps the temperature 1h.It will move back Substrate after fire is warming up to 850 DEG C, keeps the temperature 3h.Substrate after coring is warming up to 1000 DEG C, keeps the temperature 2h.Substrate is impregnated The hydrofluoric acid treatment 30min of 2.8wt%, then substrate, is finally kept the temperature 2h by supersound washing 1h at 1350 DEG C.
Embodiment 3
Choose raw material:20 parts of silica 1,10 parts of sodium oxide molybdena, 9 parts of calcium oxide, 15 parts of aluminium oxide, 5 parts of magnesia, zinc oxide 2 Part, 2.5 parts of yttria, 3.2 parts of zirconium dioxide, 2.5 parts of antimony oxide, 3 parts of phosphorus pentoxide, 3 parts of titanium dioxide.It presses Ratio is sufficiently mixed after weighing, and obtains mixture;Mixture is placed in smelting furnace and is warming up to 1680 DEG C, keeps the temperature 1.8h, then soon Rapid-result type;Substrate after molding is warming up to 200 DEG C, keeps the temperature 1h, air cooling is to room temperature, then is warming up to 250 DEG C, keeps the temperature 1h, Air cooling is to room temperature, then is warming up to 300 DEG C, keeps the temperature 1h, and air cooling to room temperature then heats to 500 DEG C, keeps the temperature 1h.It will Substrate after annealing is warming up to 850 DEG C, keeps the temperature 3h.Substrate after coring is warming up to 1000 DEG C, keeps the temperature 2h.Substrate is impregnated The hydrofluoric acid treatment 30min of 2wt%, then substrate, is finally kept the temperature 2h by supersound washing 1h at 1200 DEG C.
Substrate obtained by embodiment 1-3 after testing, Mohs' hardness >=8,1mm visible light transmittances are all higher than 80%.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field;In the present invention Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention Technical spirit still falls within the technology of the present invention side to any simple modification, change and equivalent transformation made by above example The protection domain of case.

Claims (9)

1. a kind of intelligent light-controlled glass high rigidity substrate, which is characterized in that the substrate contains following components and parts by weight:Dioxy 80-120 parts of SiClx, 10-15 parts of sodium oxide molybdena, 7-9 parts of calcium oxide, 15-20 parts of aluminium oxide, 3-5 parts of magnesia, 2-4 parts of zinc oxide, 1.5-2.5 parts of yttria, 2.8-3.2 parts of zirconium dioxide, 2.5-3.5 parts of antimony oxide, 1-3 parts of phosphorus pentoxide, two 3-5 parts of titanium oxide.
2. a kind of intelligent light-controlled glass high rigidity substrate as described in claim 1, which is characterized in that the substrate contains following Component and parts by weight:00 part of silica 1,12 parts of sodium oxide molybdena, 8 parts of calcium oxide, 18 parts of aluminium oxide, 4 parts of magnesia, zinc oxide 3 Part, 2 parts of yttria, 3 parts of zirconium dioxide, 3 parts of antimony oxide, 2 parts of phosphorus pentoxide, 4 parts of titanium dioxide.
3. a kind of preparation method of intelligent light-controlled glass high rigidity substrate described in claim 1, which is characterized in that this method It comprises the steps of:
1)Raw material is chosen, is sufficiently mixed after weighing in proportion, obtains mixture;
2)Mixture is placed in smelting furnace and is warming up to melting, keeps the temperature 1.5-2h, then rapid shaping;
3)Annealing;
4)Coring is handled;
5)Crystallizing treatment;
6)Etch is handled.
4. the preparation method of intelligent light-controlled glass high rigidity substrate as claimed in claim 3, which is characterized in that the step 2)Middle melting temperature is 1650-1700 DEG C.
5. the preparation method of intelligent light-controlled glass high rigidity substrate as claimed in claim 3, which is characterized in that the step 3)Middle annealing specific method is:Substrate after molding is warming up to 200 DEG C, keeps the temperature 1h, air cooling is to room temperature, then heats up To 250 DEG C, 1h is kept the temperature, air cooling is to room temperature, then is warming up to 300 DEG C, keeps the temperature 1h, and air cooling to room temperature then heats to 500 DEG C, keep the temperature 1h.
6. the preparation method of intelligent light-controlled glass high rigidity substrate as claimed in claim 3, which is characterized in that the step 4)Middle coring processing method is:Substrate after annealing is warming up to 850 DEG C, keeps the temperature 3h.
7. the preparation method of intelligent light-controlled glass high rigidity substrate as claimed in claim 3, which is characterized in that the step 5)Middle Crystallizing treatment method is:Substrate after coring is warming up to 1000 DEG C, keeps the temperature 2h.
8. the preparation method of intelligent light-controlled glass high rigidity substrate as claimed in claim 3, which is characterized in that the step 6)Middle etching handling method is:Substrate surface acid soak is handled into 30min, then supersound washing 1h, finally exists substrate 1200-1350 DEG C of heat preservation 2h.
9. the preparation method of intelligent light-controlled glass high rigidity substrate as claimed in claim 8, which is characterized in that the acid solution For the hydrofluoric acid of 2-2.8wt%.
CN201810607454.3A 2018-06-13 2018-06-13 A kind of intelligent light-controlled glass high rigidity substrate and preparation method thereof Pending CN108623166A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112897902A (en) * 2021-03-29 2021-06-04 晶瓷玻璃科技(上海)有限公司 Steel section system preparation method

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001048581A (en) * 1999-06-01 2001-02-20 Ohara Inc High-rigidity glass ceramic substrate
CN1974456A (en) * 2006-12-11 2007-06-06 巫汉生 Etched microcrystalline glass plate and its production process
CN103030286A (en) * 2012-12-05 2013-04-10 毛庆云 Surface dense pore-free microcrystalline glass and preparation method thereof
CN105084763A (en) * 2015-07-31 2015-11-25 安徽和润特种玻璃有限公司 Method for preparing high-tenacity high-hardness anti-dazzle glass
CN105800940A (en) * 2016-03-10 2016-07-27 温州市康尔微晶器皿有限公司 Glass ceramic with unique optical property and preparation method thereof
CN107235633A (en) * 2017-06-06 2017-10-10 梧州水森林纳米材料科技有限公司 Transparent nano crystal glass and preparation method thereof
CN107777872A (en) * 2016-08-26 2018-03-09 芜湖新利德玻璃制品有限公司 High rigidity glass and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001048581A (en) * 1999-06-01 2001-02-20 Ohara Inc High-rigidity glass ceramic substrate
CN1974456A (en) * 2006-12-11 2007-06-06 巫汉生 Etched microcrystalline glass plate and its production process
CN103030286A (en) * 2012-12-05 2013-04-10 毛庆云 Surface dense pore-free microcrystalline glass and preparation method thereof
CN105084763A (en) * 2015-07-31 2015-11-25 安徽和润特种玻璃有限公司 Method for preparing high-tenacity high-hardness anti-dazzle glass
CN105800940A (en) * 2016-03-10 2016-07-27 温州市康尔微晶器皿有限公司 Glass ceramic with unique optical property and preparation method thereof
CN107777872A (en) * 2016-08-26 2018-03-09 芜湖新利德玻璃制品有限公司 High rigidity glass and preparation method thereof
CN107235633A (en) * 2017-06-06 2017-10-10 梧州水森林纳米材料科技有限公司 Transparent nano crystal glass and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112897902A (en) * 2021-03-29 2021-06-04 晶瓷玻璃科技(上海)有限公司 Steel section system preparation method

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