LU504602B1 - Co doped luminescent colored microcrystalline glass and its preparation method - Google Patents
Co doped luminescent colored microcrystalline glass and its preparation method Download PDFInfo
- Publication number
- LU504602B1 LU504602B1 LU504602A LU504602A LU504602B1 LU 504602 B1 LU504602 B1 LU 504602B1 LU 504602 A LU504602 A LU 504602A LU 504602 A LU504602 A LU 504602A LU 504602 B1 LU504602 B1 LU 504602B1
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- microcrystalline glass
- doped luminescent
- glass
- doped
- luminescent colored
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- 239000011521 glass Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 9
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 5
- 239000010941 cobalt Substances 0.000 claims abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 5
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical group [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010411 cooking Methods 0.000 claims abstract description 4
- 230000006698 induction Effects 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002241 glass-ceramic Substances 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 229940045032 cobaltous nitrate Drugs 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- -1 lithium aluminum silicon Chemical compound 0.000 abstract description 8
- 230000007547 defect Effects 0.000 abstract description 2
- 229910008556 Li2O—Al2O3—SiO2 Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 239000010431 corundum Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 101100348017 Drosophila melanogaster Nazo gene Proteins 0.000 description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 2
- 229910000410 antimony oxide Inorganic materials 0.000 description 2
- 229910000413 arsenic oxide Inorganic materials 0.000 description 2
- 229960002594 arsenic trioxide Drugs 0.000 description 2
- 239000008395 clarifying agent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 229910052642 spodumene Inorganic materials 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 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
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal 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
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- 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
- C03C10/0018—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 containing SiO2, Al2O3 and monovalent metal oxide as main constituents
- C03C10/0027—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 containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/02—Compositions for glass with special properties for coloured glass
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/77344—Aluminosilicates
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
- F24C15/00—Details
- F24C15/02—Doors specially adapted for stoves or ranges
- F24C15/04—Doors specially adapted for stoves or ranges with transparent panels
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
- F24C15/00—Details
- F24C15/10—Tops, e.g. hot plates; Rings
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
- F24C7/00—Stoves or ranges heated by electric energy
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24C—DOMESTIC STOVES OR RANGES ; DETAILS OF DOMESTIC STOVES OR RANGES, OF GENERAL APPLICATION
- F24C7/00—Stoves or ranges heated by electric energy
- F24C7/02—Stoves or ranges heated by electric energy using microwaves
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The present invention discloses a co doped luminescent colored microcrystalline glass and its preparation method, belonging to the technical field of lithium aluminum silicon microcrystalline glass. The co doped luminescent colored microcrystalline glass is a co doped luminescent colored microcrystalline glass prepared by doping transition element and rare earth element in Li2O-Al2O3-SiO2 microcrystalline glass; the transition element is cobalt; the rare earth element is europium. The sample prepared by the present invention exhibits a bright purple color and can be excited by blue light to emit a strong red light. It not only solves the defect of single color and function of microwave oven glass panel and induction cooking panel, but also makes the products with fluorescent anti-counterfeiting function. The products provided have broad market application prospects.
Description
DESCRIPTION LU504602
CO DOPED LUMINESCENT COLORED MICROCRYSTALLINE GLASS AND ITS
PREPARATION METHOD
The present invention belongs to the technical field of lithium aluminum silicon microcrystalline glass, and specifically relates to a co doped luminescent colored microcrystalline glass and its preparation method.
With the continuous improvement of people's living standards, the pursuit of personalized products is also increasing. Taking mass consumer microwave ovens as an example, people tend to demand differentiation in their appearance. Conventional microwave oven microcrystalline glass panels are either black or milky white, with a monotonous product color that cannot meet the appearance and personalized needs of modern consumers.
At present, the production of microcrystalline glass generally requires the addition of arsenic oxide or antimony oxide as a clarifying agent, but this clarifying agent poses a pollution risk.
SUMMARY LU504602
To solve the above problems, the present invention provides a co doped luminescent colored microcrystalline glass and its preparation method. The present invention is based on the doping of transition metal ions to solve the problem of single color in microcrystalline glass panels, and improves the product formula of conventional
LioO-Al203-SiO2 microcrystalline glass. Colorful microcrystalline glass is prepared using a formula without adding arsenic oxide or antimony oxide. Further, co doping of rare earth elements enables the product to have fluorescence characteristics, enabling it to have built-in fluorescent anti-counterfeiting function and broad market application prospects.
To achieve the above objectives, the present invention provides the following technical solutions:
The first technical solution of the present invention: Providing a co doped luminescent colored microcrystalline glass, which is prepared by doping transition element and rare earth element in Li20-Al203-SiO2 microcrystalline glass; the transition element is cobalt; the rare earth element is europium.
The formula principle of the invention is: designing the glass composition according to the Li>O-Al>O3-SiO> ternary phase diagram, and adjusting the source of raw materials for some of its components on the premise that the basic components remain the same:
Li2O 2%, Al203 25%, SiO2 63%. Part of Liz2O is introduced by spodumene tailings, and appropriate mineral raw materials are used to introduce the nucleation agents TiO, P205 and ZrO.
The optical properties of rare earth ions are mainly attributed to electric dipole transitions, which are influenced by local structures around rare earth ions in glass. Rare earth element ions can selectively merge into the oxide crystal phase after heat treatment and possess low vibrational quantum energy, while obtaining precipitate crystal phase sizes smaller than visible light wavelengths to keep the material transparent. However, the co doping process can alter the local structure of rare earth ions, thereby affecting their luminescent properties. How to ensure the transparency of the material, the luminescent properties of rare earth ions, and the chromaticity 68504602 transition metal ions during the preparation process is an existing technical challenge. By precisely regulating the crystallization treatment system and doped elements, the invention enables the prepared glass ceramics to have good light transmittance, bright colors and special fluorescence effects without changing the local environment around rare earth ions, which is difficult to achieve in current production.
Preferably, the components of the Li2O-Al203-SiO2> microcrystalline glass include:
Li2O, Al203, SiOz, ZnO, BaO, TiO2, MgO, P20s, KO and NaO.
Preferably, the europium is doped in the form of EuzO3, with a doping amount of 0.2-0.7% of the total mass of the co doped luminescent colored microcrystalline glass.
Preferably, the transition element cobalt is doped in the form of cobaltous nitrate, and the doping amount is 0.5-4% of the total mass of the co doped luminescent colored glass ceramics.
The second technical solution of the present invention: Providing a preparation method for the co doped luminescent colored microcrystalline glass, comprising the following steps:
Mixing the raw materials of each component, melting them after ball milling, and pouring the obtained glass liquid into a preheated mold for molding. Then, directly performing crystallization treatment to obtain co doped luminescent colored microcrystalline glass.
Preferably, the temperature gradient of the melting is first increased to 1450 DEG C at a heating rate of 5 DEG C per minute, and after retaining its heat for 60 minutes, increasing it at a heating rate of 1 DEG C per minute to 1640 DEG C, and retaining its heat for 360 minutes.
Preferably, the crystallization treatment specifically involves retaining the heat of the sample at a temperature of 730 DEG C for 30 minutes, then raising to 920 DEG C at a heating rate of 4.5 DEG C per minute, retaining its heat for 20 minutes, naturally cooling it to room temperature, and completing crystallization.
The third technical solution of the present invention: Providing an application of tH&J504602 above co doped luminescent colored glass ceramics in the preparation of microwave oven glass panel or induction cooking panel.
The fourth technical solution of the present invention: an application of the co doped luminescent colored microcrystalline glass in fluorescent anti-counterfeiting.
The beneficial technical effects of the present invention are as follows:
The sample prepared by the present invention exhibits a bright purple color and can be excited by blue light to emit a strong red light. It not only solves the defect of single color and function of microwave oven glass panel and induction cooking panel, but also makes the products with fluorescent anti-counterfeiting function. The products provided have broad market application prospects.
Figure 1 is a photo of the microcrystalline glass prepared in embodiment 1.
Figure 2 shows the emission spectrum of the microcrystalline glass prepared in embodiment 1 under 467.5nm excitation.
Figure 3 shows the excitation spectrum of the prepared microcrystalline glass.
The various exemplary embodiments of the present invention are now explained in detail, which should not be considered as a limitation of the present invention, but should be understood as a more detailed description of certain aspects, characteristics, and implementation schemes of the present invention. It should be understood that the terms described in the present invention are only intended to describe specific embodiments and are not intended to limit the present invention.
In addition, for the numerical range in the present invention, it should be understodd/504602 that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Each smaller range between any stated value or intermediate value within the stated range, as well as any other stated value or intermediate value within the stated range, is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded from the range.
Unless otherwise stated, all technical and scientific terms used in this article have the same meanings as those commonly understood by conventional technical personnel in the field described in the present invention. Although the present invention only describes preferred methods and materials, any methods and materials similar or equivalent to those described herein can also be used in the implementation or testing of the present invention.
The terms “including”, “comprising”, “possessing”, “containing”, and so on used in this article are all open-ended terms, meaning including but not limited to.
Embodiment 1
Preparation of co doped luminescent purple microcrystalline glass:
Preparing each raw material in the proportions of Li2O, Al203, SiOz, ZnO, BaO, TiO,
MgO, P20s, KO, NaxO, C0203 and EuzO3 as shown in Table 1. The ingredient list is shown in Table 2.
Mixing all the raw materials thoroughly, mixing well, ball-milling them, melting them in a corundum crucible in a high-temperature furnace, raising them to 1450 DEG C at room temperature at 5 DEG C/min, retaining their heat for 60 minutes, and then raising them to 1640 DEG C at 1 DEG C/min, retaining their heat for 360 minutes; placing the glass liquid in a preheated mold for molding; then, the glass is placed in a muffle furnace at 730 DEG C for 30 minutes, and then heated to 920 DEG C at 4.5 DEG C/min for 20 minutes. It is naturally cooled to room temperature to obtain co doped luminescent purple microcrystalline glass.
Embodiment 2
Preparation of co doped luminescent purple microcrystalline glass:
Preparing each raw material in the proportions of Li2O, Al20s, SiO», ZnO, BaO, TiO:U504602
MgO, P20s, KO, NazO, C0203, and EuzO3 as shown in Table 1. The ingredient list is shown in Table 2.
Mixing all the raw materials thoroughly, mixing well, ball-milling them, melting them in a corundum crucible in a high-temperature furnace, raising them to 1450 DEG C at room temperature at 5 DEG C/min, retaining their heat for 60 minutes, and then raising them to 1640 DEG C at 1 DEG C/min, retaining their heat for 360 minutes; placing the glass liquid in a preheated mold for molding; then, the glass is placed in a muffle furnace at 730 DEG C for 30 minutes, and then heated to 920 DEG C at 4.5 DEG C/min for 20 minutes. It is naturally cooled to room temperature to obtain co doped luminescent purple microcrystalline glass.
Embodiment 3
Preparation of co doped luminescent purple microcrystalline glass:
Preparing each raw material in the proportions of Li2O, Al203, SiOz, ZnO, BaO, TiO,
MgO, P20s, KO, NazO, C0203, and EuzO3 as shown in Table 1. The ingredient list is shown in Table 2.
Mixing all the raw materials thoroughly, mixing well, ball-milling them, melting them in a corundum crucible in a high-temperature furnace, raising them to 1450 DEG C at room temperature at 5 DEG C/min, retaining their heat for 60 minutes, and then raising them to 1640 DEG C at 1 DEG C/min, retaining their heat for 360 minutes; placing the glass liquid in a preheated mold for molding; then, the glass is placed in a muffle furnace at 730 DEG C for 30 minutes, and then heated to 920 DEG C at 4.5 DEG C/min for 20 minutes. It is naturally cooled to room temperature to obtain co doped luminescent purple microcrystalline glass.
Embodiment 4
Preparation of co doped luminescent purple microcrystalline glass:
Preparing each raw material according to the proportions of LisO, Al.Os, SiO2, ZnO,
BaO, TiO2, MgO, P20s, KO, NazO, and Co203 shown in Table 1. The ingredient table is shown in Table 2.
Mixing all the raw materials thoroughly, mixing well, ball-milling them, melting thebJ504602 in a corundum crucible in a high-temperature furnace, raising them to 1450 DEG C at room temperature at 5 DEG C/min, retaining their heat for 60 minutes, and then raising them to 1640 DEG C at 1 DEG C/min, retaining their heat for 360 minutes; placing the glass liquid in a preheated mold for molding; then, the glass is placed in a muffle furnace at 730 DEG C for 30 minutes, and then heated to 920 DEG C at 4.5 DEG C/min for 20 minutes.
It is naturally cooled to room temperature to obtain co doped luminescent purple microcrystalline glass.
Table 1 Composition Content of Microcrystalline Glass Prepared in Embodiments 1-U504602 4 (wt. %) lo [mo [so [ror [z00 [se0 [wo
Embodiment 5.14 23.15 162.09 |2.03 1.48 0.95 0.30 1
Embodiment 5.15 23.29 162.48 | 2.05 1.49 0.30 2
Embodiment 5.52 2493 166.90 | 2.19 1.59 1.03 0.32 3
Embodiment 5.91 26.72 171.69 | 2.35 1.71 1.10 0.34 4 [neo [ko [mor (a0: [eco [000 ___
Embodiment 0.26 0.32 0.63 1.57 1.80 0.27 1
Embodiment 0.26 0.33 0.64 1.58 0.92 0.54 2
Embodiment 0.28 0.35 0.68 1.69 0.58 3
Embodiment 0.30 0.38 0.73 1.81 1.06 0.62 4
Table 2 Ingredients of the Microcrystalline Glass Prepared in Embodiments 1-4 (g}U504602
FE i
Aluminum
Eads [6% [em [ee
Spodumene
Ammonium
The parameters of the microcrystalline glass prepared in embodiments 1-4 are shown in Table 2.
Table 2 Partial Parameters of the Microcrystalline Glass Prepared in Embodiments/504602 1-4
Expansion
White Light oo Bending
Lab Chromaticity Coefficient
Transmittance Strength
Value (20-700DEG (1cm thick) (Mpa)
C/K)
Embodiment | 26.76, 2.15, 73.02 4.5107 176 1 -3.46
Embodiment > 26.93, 1.6, -2.15 | 57.83 6.4*107 174
Embodiment 3 26.16, 0.9, -1.84 | 47.08 4.8*107 178
Embodiment 4 25.63, 0.6, -1.23 | 34.42 4.2*107 182
The photo of the microcrystalline glass prepared in embodiment 1 is shown in
Figure 1.
The emission spectrum of the microcrystalline glass prepared in embodiment 1 under 467.5nm excitation is shown in Figure 2.
The excitation spectrum of the microcrystalline glass prepared in embodiment 1 is shown in Figure 3.
The emission spectra of the microcrystalline glass prepared in embodiments 2—4 under excitation are similar to those of the microcrystalline glass prepared in embodiment 1.
The above described embodiments are only a description of the preferred method of the present invention and do not limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made by ordinary technical personnel in the field to the technical solution of the present invention should fall within the scope of protection determined in the claims of the present invention.
Claims (9)
1. A co doped luminescent colored microcrystalline glass, characterized in that the co doped luminescent colored microcrystalline glass is prepared by a doping transition element and a rare earth element in Li20-Al203-SiO2 microcrystalline glass; the transition element is cobalt; the rare earth element is europium.
2. The co doped luminescent colored microcrystalline glass according to claim 1, characterized in that the components of the Li>O-Al>O3- SiO2 microcrystalline glass include: Li20, Al203, SiOz, ZnO, BaO, TiO2, MgO, P2Os, K2O and Naz0.
3. The co doped luminescent colored microcrystalline glass according to claim 1, characterized in that the europium is doped in the form of Euz»O3, with a doping amount of 0.2-0.7% of the total mass of the co doped luminescent colored microcrystalline glass.
4. The co doped luminescent colored glass ceramics according to claim 1, which is characterized in that the transition element cobalt is doped in the form of cobaltous nitrate, and the doping amount is 0.5-4% of the total mass of the co doped luminescent colored glass ceramics.
5. A preparation method for co doped luminescent colored microcrystalline glass according to any one of claims 1-4, characterized in that it comprises the following steps: mixing the raw materials of each component, melting them after ball milling, and pouring the obtained glass liquid into a preheated mold for molding, and then directly performing crystallization treatment to obtain co doped luminescent colored microcrystalline glass.
6. The preparation method according to claim 5, characterized in that tH&J504602 temperature gradient of the melting is first increased to 1450 DEG C at a heating rate of DEG C per minute, and after retaining its heat for 60 minutes, increasing it at a heating rate of 1 DEG C per minute to 1640 DEG C, and retaining its heat for 360 minutes.
7. The preparation method according to claim 5, characterized in that the crystallization treatment specifically involves retaining the heat of the sample at a temperature of 730 DEG C for 30 minutes, then raising to 920 DEG C at a heating rate of
4.5 DEG C per minute, retaining its heat for 20 minutes, naturally cooling it to room temperature, and completing crystallization.
8. An application of the co doped luminescent colored microcrystalline glass in preparation of microwave oven glass panel or induction cooking panel, as claimed in any one of claims 1-4
9. An application of the co doped luminescent colored microcrystalline glass in fluorescent anti-counterfeiting, as claimed in any one of claims 1-4.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310674116.2A CN116693199A (en) | 2023-06-08 | 2023-06-08 | Co-doped luminous color glass ceramic and preparation method thereof |
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| LU504602B1 true LU504602B1 (en) | 2024-01-09 |
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| LU504602A LU504602B1 (en) | 2023-06-08 | 2023-06-28 | Co doped luminescent colored microcrystalline glass and its preparation method |
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| LU (1) | LU504602B1 (en) |
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