CN116693199A - Co-doped luminous color glass ceramic and preparation method thereof - Google Patents
Co-doped luminous color glass ceramic and preparation method thereof Download PDFInfo
- Publication number
- CN116693199A CN116693199A CN202310674116.2A CN202310674116A CN116693199A CN 116693199 A CN116693199 A CN 116693199A CN 202310674116 A CN202310674116 A CN 202310674116A CN 116693199 A CN116693199 A CN 116693199A
- Authority
- CN
- China
- Prior art keywords
- luminescent color
- doped
- color glass
- glass
- doped luminescent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 32
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 14
- 230000007704 transition Effects 0.000 claims abstract description 9
- 229910008556 Li2O—Al2O3—SiO2 Inorganic materials 0.000 claims abstract description 8
- 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
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000001816 cooling Methods 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 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- -1 lithium aluminum silicon Chemical compound 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 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
- 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
- 239000000203 mixture Substances 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 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 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 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
- 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
- 229910052642 spodumene Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 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
Landscapes
- 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)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind ofA co-doped luminous color glass ceramic and a preparation method thereof, belonging to the technical field of lithium aluminum silicon glass ceramic. The co-doped luminescent color glass ceramic is Li 2 O‑Al 2 O 3 ‑SiO 2 The co-doped luminescent color glass ceramics are prepared by doping transition elements and rare earth elements into glass ceramics; the transition element is cobalt; the rare earth element is europium. The sample prepared by the invention has bright purple color and can be excited by blue light to emit intense red light. Not only solves the defects of single color and function of the glass panel and the electromagnetic oven panel of the microwave oven, but also ensures that the product has a fluorescent anti-counterfeiting function, and the provided product has wide market application prospect.
Description
Technical Field
The invention belongs to the technical field of lithium aluminum silicon microcrystalline glass, and particularly relates to co-doped luminous color microcrystalline glass and a preparation method thereof.
Background
Along with the continuous improvement of the living standard of people, the pursuit of personalized products is also higher and higher. Taking the example of a consumer microwave oven, there is a greater tendency to require a differentiation in the appearance. The conventional glass ceramic panel of the microwave oven is black or milky, the color of the product is monotonous, and the requirements of modern consumers on appearance and individuation are difficult to meet.
At present, arsenic oxide or antimony oxide is generally required to be added for producing microcrystalline glass as a clarifying agent, but the clarifying agent has pollution risk.
Disclosure of Invention
In order to solve the problems, the invention provides co-doped luminescent color glass ceramics and a preparation method thereof. The invention is based on the problem of single color of the microcrystalline glass panel by doping transition metal ions, improves the conventional Li 2 O-Al 2 O 3 -SiO 2 The microcrystalline glass is prepared by adopting a formula without arsenic oxide or antimony oxide. The product has fluorescence property by further co-doping rare earth elements, so that the product is self-fluorescenceThe light anti-counterfeiting function has wide market application prospect.
In order to achieve the above purpose, the present invention provides the following technical solutions:
one of the technical schemes of the invention is as follows: provides co-doped luminous color microcrystalline glass which is Li 2 O-Al 2 O 3 -SiO 2 The co-doped luminescent color glass ceramics are prepared by doping transition elements and rare earth elements into glass ceramics; the transition element is cobalt; the rare earth element is europium.
The formula principle of the invention is as follows: according to Li 2 O-Al 2 O 3 -SiO 2 Designing glass composition by ternary phase diagram, and Li under the premise of unchanged basic components 2 O 2％，Al 2 O 3 25％，SiO 2 63%, adjusting the source of part of the component raw materials and part of Li 2 O is introduced by spodumene tailings, and a proper mineral raw material is introduced into a crystal nucleus agent TiO 2 、P 2 O 5 ZrO (ZrO) 2 。
The optical properties of rare earth ions are mainly due to the galvanic transitions, which are affected by the local structure around the rare earth ions in the glass. Rare earth ions can be selectively incorporated into the oxide crystal phase after heat treatment and possess low vibration quantum energy while achieving a precipitate crystal phase size smaller than the wavelength of visible light to maintain transparency of the material. However, the co-doping process can change the local structure of the rare earth ions so as to influence the luminous performance of the rare earth ions, and how to ensure the transparency of the material, the luminous performance of the rare earth ions and the color-forming property of the transition metal ions in the preparation process is a prior technical difficulty. According to the invention, through accurate regulation and control of crystallization treatment system and doping elements, the prepared glass ceramics has good light transmittance, bright color and special fluorescent effect under the condition of not changing local environment around rare earth ions, and the technology is difficult to realize in the current production.
Preferably, the Li 2 O-Al 2 O 3 -SiO 2 The microcrystalline glass comprises the following components: li (Li) 2 O、Al 2 O 3 、SiO 2 、ZnO、BaO、TiO 2 、MgO、P 2 O 5 、K 2 O and Na 2 O。
Preferably, the europium is Eu 2 O 3 The doping amount is 0.2 to 0.7 percent of the total mass of the co-doped luminescent color glass ceramic.
Preferably, the transition element cobalt is doped in the form of cobalt nitrate, and the doping amount is 0.5-4% of the total mass of the co-doped luminescent color glass ceramic.
The second technical scheme of the invention is as follows: the preparation method of the co-doped luminescent color glass ceramic comprises the following steps:
mixing the raw materials of the components, ball milling, melting, pouring the obtained glass liquid into a preheated mold for molding, and then directly carrying out crystallization treatment to obtain the co-doped luminescent color glass ceramics.
Preferably, the temperature gradient of the melting is that the temperature is firstly increased to 1450 ℃ at a heating rate of 5 ℃/min, then is increased to 1640 ℃ at a heating rate of 1 ℃/min after being kept for 60min, and is kept for 360min.
Preferably, the crystallization treatment is specifically to keep the sample at 730 ℃ for 30min, then raise the temperature to 920 ℃ at a heating rate of 4.5 ℃/min, keep the temperature for 20min, and naturally cool to room temperature to finish crystallization.
The third technical scheme of the invention: the application of the co-doped luminescent color glass ceramic in preparing a glass panel of a microwave oven or a panel of an electromagnetic oven is provided.
The fourth technical scheme of the invention: the application of the co-doped luminescent color glass ceramic in fluorescence anti-counterfeiting.
The beneficial technical effects of the invention are as follows:
the sample prepared by the invention has bright purple color and can be excited by blue light to emit intense red light. Not only solves the defects of single color and function of the glass panel and the electromagnetic oven panel of the microwave oven, but also ensures that the product has a fluorescent anti-counterfeiting function, and the provided product has wide market application prospect.
Drawings
FIG. 1 is a photograph of glass ceramics prepared in example 1.
FIG. 2 is a graph showing the emission spectrum of the glass-ceramic prepared in example 1 under 467.5nm excitation.
FIG. 3 is an excitation spectrum of the glass-ceramic.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
Preparing co-doped luminescent purple microcrystalline glass:
according to Li shown in Table 1 2 O、Al 2 O 3 、SiO 2 、ZnO、BaO、TiO 2 、MgO、P 2 O 5 、K 2 O、Na 2 O、Co 2 O 3 And Eu 2 O 3 The proportions of the raw materials are shown in Table 2.
Mixing the raw materials, fully stirring, uniformly mixing, ball milling, putting into a corundum crucible, melting in a high-temperature furnace, heating to 1450 ℃ at a speed of 5 ℃/min at room temperature, preserving heat for 60min, heating to 1640 ℃ at a speed of 1 ℃/min, and preserving heat for 360min; placing the glass liquid into a preheated mold for molding; then placing the glass into a muffle furnace with 730 ℃ for heat preservation for 30min, heating to 920 ℃ at 4.5 ℃/min for heat preservation for 20min, and naturally cooling to room temperature to obtain the co-doped luminescent purple microcrystalline glass.
Example 2
Preparing co-doped luminescent purple microcrystalline glass:
according to Li shown in Table 1 2 O、Al 2 O 3 、SiO 2 、ZnO、BaO、TiO 2 、MgO、P 2 O 5 、K 2 O、Na 2 O、Co 2 O 3 And Eu 2 O 3 The proportions of the raw materials are shown in Table 2.
Mixing the raw materials, fully stirring, uniformly mixing, ball milling, putting into a corundum crucible, melting in a high-temperature furnace, heating to 1450 ℃ at a speed of 5 ℃/min at room temperature, preserving heat for 60min, heating to 1640 ℃ at a speed of 1 ℃/min, and preserving heat for 360min; placing the glass liquid into a preheated mold for molding; then placing the glass into a muffle furnace with 730 ℃ for heat preservation for 30min, heating to 920 ℃ at 4.5 ℃/min for heat preservation for 20min, and naturally cooling to room temperature to obtain the co-doped luminescent purple microcrystalline glass.
Example 3
Preparing co-doped luminescent purple microcrystalline glass:
according to Li shown in Table 1 2 O、Al 2 O 3 、SiO 2 、ZnO、BaO、TiO 2 、MgO、P 2 O 5 、K 2 O、Na 2 O、Co 2 O 3 And Eu 2 O 3 The proportions of the raw materials are shown in Table 2.
Mixing the raw materials, fully stirring, uniformly mixing, ball milling, putting into a corundum crucible, melting in a high-temperature furnace, heating to 1450 ℃ at a speed of 5 ℃/min at room temperature, preserving heat for 60min, heating to 1640 ℃ at a speed of 1 ℃/min, and preserving heat for 360min; placing the glass liquid into a preheated mold for molding; then placing the glass into a muffle furnace with 730 ℃ for heat preservation for 30min, heating to 920 ℃ at 4.5 ℃/min for heat preservation for 20min, and naturally cooling to room temperature to obtain the co-doped luminescent purple microcrystalline glass.
Example 4
Preparing co-doped luminescent purple microcrystalline glass:
according to Li shown in Table 1 2 O、Al 2 O 3 、SiO 2 、ZnO、BaO、TiO 2 、MgO、P 2 O 5 、K 2 O、Na 2 O and Co 2 O 3 The proportions of the raw materials are shown in Table 2.
Mixing the raw materials, fully stirring, uniformly mixing, ball milling, putting into a corundum crucible, melting in a high-temperature furnace, heating to 1450 ℃ at a speed of 5 ℃/min at room temperature, preserving heat for 60min, heating to 1640 ℃ at a speed of 1 ℃/min, and preserving heat for 360min; placing the glass liquid into a preheated mold for molding; then placing the glass into a muffle furnace with 730 ℃ for heat preservation for 30min, heating to 920 ℃ at 4.5 ℃/min for heat preservation for 20min, and naturally cooling to room temperature to obtain the co-doped luminescent purple microcrystalline glass.
Table 1 component content (wt.%) of the glass ceramics prepared in examples 1 to 4
| Li 2 O | Al 2 O 3 | SiO 2 | TiO 2 | ZnO | BaO | MgO | |
| Example 1 | 5.14 | 23.15 | 62.09 | 2.03 | 1.48 | 0.95 | 0.30 |
| Example 2 | 5.15 | 23.29 | 62.48 | 2.05 | 1.49 | 0.96 | 0.30 |
| Example 3 | 5.52 | 24.93 | 66.90 | 2.19 | 1.59 | 1.03 | 0.32 |
| Example 4 | 5.91 | 26.72 | 71.69 | 2.35 | 1.71 | 1.10 | 0.34 |
| Na 2 O | K 2 O | P 2 O 5 | ZrO 2 | Eu 2 O 3 | Co 2 O 3 | ||
| Example 1 | 0.26 | 0.32 | 0.63 | 1.57 | 1.80 | 0.27 | |
| Example 2 | 0.26 | 0.33 | 0.64 | 1.58 | 0.92 | 0.54 | |
| Example 3 | 0.28 | 0.35 | 0.68 | 1.69 | 0.99 | 0.58 | |
| Example 4 | 0.30 | 0.38 | 0.73 | 1.81 | 1.06 | 0.62 |
TABLE 2 formulation (g) of glass ceramics prepared in examples 1-4
The parameters of the glass ceramics obtained in examples 1 to 4 are shown in Table 2.
TABLE 2 partial parameters of the glass ceramics obtained in examples 1 to 4
The photo of the glass ceramics prepared in example 1 is shown in FIG. 1.
The emission spectrum of the glass ceramics prepared in example 1 under 467.5nm excitation is shown in FIG. 2.
The excitation spectrum of the glass ceramics prepared in example 1 is shown in FIG. 3.
The emission spectra of the glass ceramics prepared in examples 2 to 4 under excitation were similar to those of the glass ceramics prepared in example 1.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (9)
1. A co-doped luminous color glass ceramic is characterized in that Li 2 O-Al 2 O 3 -SiO 2 The co-doped luminescent color glass ceramics are prepared by doping transition elements and rare earth elements into glass ceramics; the transition element is cobalt; the rare earth element is europium.
2. The co-doped luminescent color glass ceramic according to claim 1, wherein the Li 2 O-Al 2 O 3 -SiO 2 The microcrystalline glass comprises the following components: li (Li) 2 O、Al 2 O 3 、SiO 2 、ZnO、BaO、TiO 2 、MgO、P 2 O 5 、K 2 O and Na 2 O。
3. The co-doped luminescent color glass ceramic according to claim 1, wherein europium is Eu 2 O 3 The doping amount is 0.2 to 0.7 percent of the total mass of the co-doped luminescent color glass ceramic.
4. The co-doped luminescent color glass-ceramic according to claim 1, wherein the transition element cobalt is doped in the form of cobalt nitrate, and the doping amount is 0.5-4% of the total mass of the co-doped luminescent color glass-ceramic.
5. A method for preparing co-doped luminescent color glass ceramics according to any one of claims 1 to 4, comprising the following steps:
mixing the raw materials of the components, ball milling, melting, pouring the obtained glass liquid into a preheated mold for molding, and then directly carrying out crystallization treatment to obtain the co-doped luminescent color glass ceramics.
6. The method according to claim 5, wherein the melting temperature gradient is raised to 1450 ℃ at a heating rate of 5 ℃/min, and is maintained for 60min, then raised to 1640 ℃ at a heating rate of 1 ℃/min, and is maintained for 360min.
7. The method according to claim 5, wherein the crystallization is performed by heating the sample at 730 ℃ for 30min, heating to 920 ℃ at a heating rate of 4.5 ℃/min, heating for 20min, and naturally cooling to room temperature.
8. Use of a co-doped luminescent color glass ceramic according to any one of claims 1 to 4 for the preparation of a glass panel for a microwave oven or a panel for an electromagnetic oven.
9. Use of a co-doped luminescent color glass ceramic according to any one of claims 1 to 4 in fluorescent anti-counterfeiting.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310674116.2A CN116693199A (en) | 2023-06-08 | 2023-06-08 | Co-doped luminous color glass ceramic and preparation method thereof |
| LU504602A LU504602B1 (en) | 2023-06-08 | 2023-06-28 | Co doped luminescent colored microcrystalline glass and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310674116.2A CN116693199A (en) | 2023-06-08 | 2023-06-08 | Co-doped luminous color glass ceramic and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116693199A true CN116693199A (en) | 2023-09-05 |
Family
ID=87836903
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310674116.2A Pending CN116693199A (en) | 2023-06-08 | 2023-06-08 | Co-doped luminous color glass ceramic and preparation method thereof |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN116693199A (en) |
| LU (1) | LU504602B1 (en) |
-
2023
- 2023-06-08 CN CN202310674116.2A patent/CN116693199A/en active Pending
- 2023-06-28 LU LU504602A patent/LU504602B1/en active
Also Published As
| Publication number | Publication date |
|---|---|
| LU504602B1 (en) | 2024-01-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104961343B (en) | Separate out NaYF4Nanocrystalline rear-earth-doped devitrified glass and preparation method thereof | |
| JP5738190B2 (en) | Transparent colored cooktop having improved color display capability and method for producing cooktop | |
| EP2817269B9 (en) | Transparent low-colour lithium aluminium silicate glass ceramic and the use thereof | |
| CN102503122B (en) | Leadless, cadmium-free and strontium-free glass and manufacture process thereof | |
| RU2396220C2 (en) | Green glass composition and its application | |
| CN106477877B (en) | Extra-high refraction high density environment-friendly type cameo glass of one kind and preparation method thereof | |
| JP2001316128A (en) | Pale colored high transmittance plate-glass and method for manufacturing same | |
| CN103396007B (en) | A kind of white light led fluorescent glass sheet and preparation method thereof | |
| WO2022151610A1 (en) | Colored microcrystalline glass and preparation method therefor | |
| WO2023035704A1 (en) | Preparation method for fluorescent lithium silicate glass ceramic | |
| CN105948514A (en) | Method for manufacturing colorful transparent colored glass ceramics with high degree of crystallinity by adopting fusing-cooling method for crystallization | |
| CN107777873B (en) | Light guide plate glass and preparation method thereof | |
| JP2003146695A (en) | Optical colored glass, method of using the same, and optical sharp edge filter | |
| CN104909562B (en) | A kind of environmentally friendly ruby glass of high refraction and preparation method | |
| CN112010553B (en) | Silicate-series ultraviolet-proof neodymium glass and preparation method thereof | |
| CN116693199A (en) | Co-doped luminous color glass ceramic and preparation method thereof | |
| CN107986618B (en) | High-strain-point aluminosilicate glass with high resistance characteristic | |
| CN114014538B (en) | Silicate glass and preparation method and application thereof | |
| CN112028478B (en) | Silicate-series anti-dazzle neodymium glass and preparation method thereof | |
| CN115772001A (en) | Color transparent glass composition, microcrystalline glass and preparation method thereof | |
| CN108164134A (en) | A kind of aubergine glass | |
| CN114804623B (en) | Cesium-lead-halide nanocrystalline dispersion glass and heat treatment method thereof | |
| CN107129144B (en) | Formula and preparation method of lead-free fusible golden red glass | |
| JP7339667B2 (en) | Crystallized glass and its manufacturing method | |
| TW202404915A (en) | Crystallized glass and method for manufacturing same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |