CN118026527A - Flexible glass suitable for down-draw production and preparation method thereof - Google Patents
Flexible glass suitable for down-draw production and preparation method thereof Download PDFInfo
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- CN118026527A CN118026527A CN202410048137.8A CN202410048137A CN118026527A CN 118026527 A CN118026527 A CN 118026527A CN 202410048137 A CN202410048137 A CN 202410048137A CN 118026527 A CN118026527 A CN 118026527A
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- 239000011521 glass Substances 0.000 title claims abstract description 95
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 37
- 238000002844 melting Methods 0.000 claims abstract description 23
- 230000008018 melting Effects 0.000 claims abstract description 23
- 238000003280 down draw process Methods 0.000 claims abstract description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 9
- 229910018068 Li 2 O Inorganic materials 0.000 claims abstract description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 4
- 229910011763 Li2 O Inorganic materials 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 238000011534 incubation Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- 239000005354 aluminosilicate glass Substances 0.000 abstract description 2
- 239000005368 silicate glass Substances 0.000 abstract description 2
- 229910052783 alkali metal Inorganic materials 0.000 abstract 1
- 150000001340 alkali metals Chemical class 0.000 abstract 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 abstract 1
- 150000001342 alkaline earth metals Chemical class 0.000 abstract 1
- 238000004321 preservation Methods 0.000 description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- 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
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses flexible glass suitable for production by a down-draw method and a preparation method thereof, and belongs to the technical field of glass preparation. The material is prepared from the following raw materials in percentage by mass: 58-68% of SiO 2, 8-15% of Al 2O3, 1-6% of MgO, 10-15% of Na 2 O, 2-5% of K 2 O, 1-5% of CaO, 0.1-0.8% of ZrO 2, 0.1-0.8% of TiO 2, 0.1-0.8% of La 2O3, 0.1-0.8% of Y 2O3 and 0.5-3.5% of Li 2 O. The prepared glass belongs to aluminosilicate glass, and the strength and toughness of the obtained flexible glass are higher than those of common silicate glass; the prepared glass has high flexibility, strong stability and excellent performance by adding alkali metal and alkaline earth metal in different proportions, and the prepared glass has lower melting temperature and forming temperature and has important application value in the technical field of flexible glass.
Description
Technical Field
The invention belongs to the technical field of glass preparation, and particularly relates to flexible glass suitable for down-draw production and a preparation method thereof.
Background
Development of intelligent electronic products such as foldable smart phones and bendable electronic wearable devices and curved surface display technology has put forward higher requirements on flexible displays. The flexible glass (UTG) is ultrathin glass with the thickness less than or equal to 0.1mm, is a core material of a foldable display device, has the characteristics of ultrathin property, wear resistance, high strength, bending property and the like, and is an important new development direction of a flexible folding cover plate. The production method of the flexible glass can be divided into a one-time molding method and a secondary processing method. The secondary processing technology of 'glass raw sheet plus chemical thinning' has the problems of low product yield, small size, waste of raw materials, acid involvement and the like. The one-step forming process mainly comprises a down-draw method, including a slit down-draw method, an overflow down-draw method and a waterfall down-draw method, the down-draw method has simple flow, the surface quality of the produced flexible glass is high, the continuous production of the glass ribbon can be realized, the yield is high, the environment-friendly type glass is strong, the flexible glass with larger breadth size and higher strength is easy to produce, and the requirements of the market on the flexible glass are met. However, the prior down-draw method has a plurality of problems in the production process, such as higher melting temperature, difficult melting of raw materials, high viscosity, difficult drawing and the like. Because flexible glass needs to meet both strength and toughness requirements, current glass materials do not have both high strength and high toughness, and therefore, the relationship between glass compositions needs to be studied to balance toughness and strength to meet the application of flexible products. Therefore, research into flexible glass suitable for down-draw production is of great value in the glass manufacturing field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides flexible glass suitable for down-draw production and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
a flexible glass suitable for down-draw production is prepared from the following raw materials in percentage by mass:
58-68% of SiO 2, 8-15% of Al 2O3, 1-6% of MgO, 10-15% of Na 2 O, 2-5% of K 2 O, 1-5% of CaO, 0.1-0.8% of ZrO 2, 0.1-0.8% of TiO 2, 0.1-0.8% of La 2O3, 0.1-0.8% of Y 2O3 and 0.5-3.5% of Li 2 O.
Further, the flexible glass suitable for production by a down-draw method is characterized in that the mass ratio of the raw materials meets the following conditions:
Na 2O+K2O+Li2 O is more than or equal to 15% and less than or equal to 20%, and Na 2O:K2 O is more than or equal to 2 and less than or equal to 5;
1≤Al2O3:(CaO+MgO+La2O3+Y2O3)≤2；
0.5％≤ZrO2+TiO2≤1％;0.5％≤La2O3+Y2O3≤1％。
a method of making a flexible glass suitable for down-draw production, comprising the steps of:
s1, uniformly mixing raw materials, and adding the raw materials into a platinum crucible for melting;
S2, casting the melted glass into a copper mold, putting the cast glass into an annealing furnace, controlling according to an annealing curve during annealing, cooling to room temperature along with the furnace after the annealing, and taking out to obtain the flexible glass suitable for down-draw production.
Further, in the step S1, the melting temperature is 1580-1650 ℃ and the heat preservation time is 3h.
Further, in the step S2, the annealing temperature is 580-680 ℃, and the heat preservation time is 1h.
The invention has the beneficial effects that:
1. The glass prepared by the invention belongs to aluminosilicate glass, and ensures that the strength and toughness of the obtained flexible glass are higher than those of common silicate glass;
2. CaO is added, and the content of CaO is controlled, so that the viscosity of the glass can be reduced, the glass is promoted to be melted and clarified, and the chemical stability and flexibility of the glass are improved;
3. The addition of Y 2O3 can effectively reduce the melting and clarifying temperature and the forming and thinning temperature of the glass, and can improve the elastic modulus of the glass so as to enhance the flexibility of the glass;
4. MgO is added, so that the high-temperature viscosity of the glass can be reduced, and the crystallization performance of the glass can be improved;
5. ZrO 2 and TiO 2 are added to improve the strength of the glass, and meanwhile, the glass structure can be optimized and the performance can be improved in the annealing process;
6. The addition of Li 2 O can obviously reduce the melting temperature of the glass, can improve the internal structure lifting performance of the glass under certain conditions, but can also increase the crystallization tendency of the glass;
7. La 2O3 is added as an important rare earth oxide, which can reduce the melting temperature and forming temperature of the glass, reduce the generation of tiny bubbles, enhance the strength of the glass, and reduce the surface tension of the glass.
Therefore, the prepared glass has high flexibility, strong stability, good clarification effect, excellent performance, lower melting temperature and forming temperature, low viscosity, suitability for down-draw production and important application value in the technical field of flexible glass.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Weighing the following raw materials in percentage by mass:
58% SiO 2, 13% Al 2O3, 4.2% MgO, 14% Na 2 O, 3% K 2 O, 5% CaO, 0.4% ZrO 2, 0.1% TiO 2, 0.6% La 2O3, 0.2% Y 2O3, 1.5% Li 2 O. In this example, the raw material was Li 2O、Na2O、K2 O, and in actual use, the raw material was Li 2CO3、Na2CO3、K2CO3.
S1, uniformly mixing the raw materials, adding the mixture into a platinum crucible for melting, wherein the melting temperature is 1610 ℃, and the heat preservation time is 3 hours;
S2, casting the melted glass into a copper mold, and placing the cast glass into an annealing furnace, wherein the annealing temperature is 580 ℃ and the heat preservation time is 1h according to an annealing curve during annealing. And after the process is finished, cooling the glass to room temperature along with the furnace, and taking out the glass to obtain the flexible glass suitable for production by a down-draw method.
Example 2
Weighing the following raw materials in percentage by mass:
64% SiO 2, 12% Al 2O3, 2.5% MgO, 12% Na 2 O, 2.5% K 2 O, 3.3% CaO, 0.2% ZrO 2, 0.6% TiO 2, 0.4% La 2O3, 0.5% Y 2O3, 2% Li 2 O. In this example, the raw material was Li 2O、Na2O、K2 O, and in actual use, the raw material was Li 2CO3、Na2CO3、K2CO3.
S1, uniformly mixing the raw materials, adding the mixture into a platinum crucible for melting, wherein the melting temperature is 1610 ℃, and the heat preservation time is 3 hours;
S2, casting the melted glass into a copper mold, and placing the cast glass into an annealing furnace, wherein the annealing temperature is 630 ℃ and the heat preservation time is 1h according to an annealing curve during annealing. And after the process is finished, cooling the glass to room temperature along with the furnace, and taking out the glass to obtain the flexible glass suitable for production by a down-draw method.
Example 3
Weighing the following raw materials in percentage by mass:
67% SiO 2%, 8% Al 2O3, 3.5% MgO, 10% Na 2 O, 5% K 2 O, 1.5% CaO, 0.5% ZrO 2, 0.5% TiO 2, 0.7% La 2O3, 0.3% Y 2O3, 3% Li 2 O. In this example, the raw material was Li 2O、Na2O、K2 O, and in actual use, the raw material was Li 2CO3、Na2CO3、K2CO3.
S1, uniformly mixing the raw materials, adding the raw materials into a platinum crucible for melting, wherein the melting temperature is 1600 ℃, and the heat preservation time is 3 hours;
S2, casting the melted glass into a copper mold, and placing the cast glass into an annealing furnace, wherein the annealing temperature is 680 ℃ and the heat preservation time is 1h according to an annealing curve during annealing. And after the process is finished, cooling the glass to room temperature along with the furnace, and taking out the glass to obtain the flexible glass suitable for production by a down-draw method.
Comparative example 1
Weighing the following raw materials in percentage by mass:
63% SiO 2, 15% Al 2O3, 2.7% MgO, 11% Na 2 O, 4% K 2 O, 2% CaO, 0.7% ZrO 2, 0.4% TiO 2, 0.1% La 2O3, 0.1% Y 2O3, 1% Li 2 O. In this example, the raw material was Li 2O、Na2O、K2 O, and in actual use, the raw material was Li 2CO3、Na2CO3、K2CO3.
S1, uniformly mixing the raw materials, adding the mixture into a platinum crucible for melting, wherein the melting temperature is 1620 ℃, and the heat preservation time is 3 hours;
S2, casting the melted glass into a copper mold, and placing the cast glass into an annealing furnace, wherein the annealing temperature is 650 ℃ and the heat preservation time is 1h according to an annealing curve during annealing. And after the process is finished, cooling the glass to room temperature along with the furnace, and taking out the glass to obtain the flexible glass suitable for production by a down-draw method.
Comparative example 2
Weighing the following raw materials in percentage by mass:
67% of SiO 2, 12% of Al 2O3, 2.5% of MgO, 12% of Na 2 O, 2.5% of K 2 O and 4% of CaO. In this example, the raw material is Na 2O、K2 O, and in actual production, the raw material is Na 2CO3、K2CO3.
S1, uniformly mixing the raw materials, adding the mixture into a platinum crucible for melting, wherein the melting temperature is 1630 ℃, and the heat preservation time is 3 hours;
S2, casting the melted glass into a copper mold, and placing the cast glass into an annealing furnace, wherein the annealing temperature is 680 ℃ and the heat preservation time is 1h according to an annealing curve during annealing. And after the process is finished, cooling the glass to room temperature along with the furnace, and taking out the glass to obtain the flexible glass suitable for production by a down-draw method.
Comparative example 3
Weighing the following raw materials in percentage by mass:
67% of SiO 2, 12% of Al 2O3, 2.5% of MgO, 12% of Na 2 O, 2.5% of K 2 O, 3.8% of CaO and 0.2% of ZrO 2. In this example, the raw material is Na 2O、K2 O, and in actual production, the raw material is Na 2CO3、K2CO3.
S1, uniformly mixing the raw materials, adding the raw materials into a platinum crucible for melting, wherein the melting temperature is 1640 ℃, and the heat preservation time is 3 hours;
S2, casting the melted glass into a copper mold, and placing the cast glass into an annealing furnace, wherein the annealing temperature is 650 ℃ and the heat preservation time is 1h according to an annealing curve during annealing. And after the process is finished, cooling the glass to room temperature along with the furnace, and taking out the glass to obtain the flexible glass suitable for production by a down-draw method.
The glasses obtained in examples 1-3 and comparative examples 1-3 were subjected to the following performance tests according to different test criteria:
The surface tension is measured by adopting the national standard GB/T39797-2021 'glass melt surface tension test method base drop method';
the elastic modulus is measured by adopting the national standard GB/T37788-2019 ultra-thin glass elastic modulus test method;
The fracture toughness is measured by adopting national standard GB/T37900-2019 'ultra-thin glass hardness and fracture toughness test method small load Vickers hardness indentation method';
The glass compositions and measured results are shown in the following table:
The glass prepared by the method has high flexibility, strong stability, excellent performance and lower forming temperature, is suitable for production by a down-draw method, and has important application value in the technical field of flexible glass.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (5)
1. The flexible glass suitable for the down-draw production is characterized by being prepared from the following raw materials in percentage by mass:
58-68% of SiO 2, 8-15% of Al 2O3, 1-6% of MgO, 10-15% of Na 2 O, 2-5% of K 2 O, 1-5% of CaO, 0.1-0.8% of ZrO 2, 0.1-0.8% of TiO 2, 0.1-0.8% of La 2O3, 0.1-0.8% of Y 2O3 and 0.5-3.5% of Li 2 O.
2. The flexible glass suitable for production by the downdraw process according to claim 1, wherein the mass ratio of the raw materials satisfies the following conditions:
Na 2O+K2O+Li2 O is more than or equal to 15% and less than or equal to 20%, and Na 2O:K2 O is more than or equal to 2 and less than or equal to 5;
1≤Al2O3:(CaO+MgO+La2O3+Y2O3)≤2；
0.5％≤ZrO2+TiO2≤1％;0.5％≤La2O3+Y2O3≤1％。
3. A method of producing a flexible glass suitable for down-draw production according to any one of claims 1-2, comprising the steps of:
s1, uniformly mixing raw materials, and adding the raw materials into a platinum crucible for melting;
S2, casting the melted glass into a copper mold, putting the cast glass into an annealing furnace, controlling according to an annealing curve during annealing, cooling to room temperature along with the furnace after the annealing, and taking out to obtain the flexible glass suitable for down-draw production.
4. The method according to claim 3, wherein the melting temperature in the step S1 is 1580℃to 1650℃and the holding time is 3 hours.
5. A method of producing a flexible glass suitable for down-draw production according to claim 3, wherein the annealing temperature in step S2 is 580 ℃ -680 ℃ and the incubation time is 1h.
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