CN116693205A - Preparation method and application of copper halide glass fluorescent material - Google Patents

Preparation method and application of copper halide glass fluorescent material Download PDF

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Publication number
CN116693205A
CN116693205A CN202310670482.0A CN202310670482A CN116693205A CN 116693205 A CN116693205 A CN 116693205A CN 202310670482 A CN202310670482 A CN 202310670482A CN 116693205 A CN116693205 A CN 116693205A
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Prior art keywords
glass
copper halide
fluorescent material
melting
copper
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CN202310670482.0A
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Inventor
陈海杰
马雪晴
周蓓莹
王连军
江莞
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Donghua University
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Donghua University
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Priority to CN202310670482.0A priority Critical patent/CN116693205A/en
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    • 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
    • C03C12/00—Powdered glass; Bead compositions
    • 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
    • C03B5/235—Heating the glass
    • 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
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
    • 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
    • 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

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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 relates to a preparation method and application of a copper halide glass fluorescent material, comprising the following steps: fully mixing a copper halide raw material with a glass raw material, sealing the mixture in a quartz tube, and vacuumizing the system; melting and quenching the mixed material at a vacuum high temperature; melting the mixed material at a high temperature to form glass liquid; and rapidly transferring and annealing the molten glass liquid to form a composite material of copper halide and glass. The invention prepares the composite system by a vacuum solid phase method, ensures Cu + Will not oxidize. Wherein the CuCl and the boron oxide glass are compoundedThe composite material integrally shows the characteristics of white light emission and yellow light emission, and the composite material of CuCl, csCl and boron oxide glass integrally shows the characteristics of green light emission.

Description

Preparation method and application of copper halide glass fluorescent material
Technical Field
The invention relates to the technical field of glass melting-quenching preparation, mainly relates to the field of preparation methods of fluorescent powder and glass composite materials, and particularly relates to a preparation method and application of a copper halide glass fluorescent material.
Background
All-inorganic metal halide perovskite materials have become a hot spot for research in recent years due to their excellent photoelectric properties and wide application prospects. They find application in information storage, solid state lighting, perovskite solar cells, scintillators, lasers, x-ray imaging screens, and many other applications. To meet the increasing demand for photovoltaic materials, the requirements for material properties are also becoming more stringent. Metal halide systems exhibit poor thermal stability, which limits their long-term function and commercial potential. Researchers have been exploring the incorporation of metal halides into glass as a potential solution to the problem of poor thermal stability. The production process of the metal halide/glass composite material includes melt quenching or sol-gel techniques to form a glass matrix. Subsequent treatments, such as quenching and femtosecond laser irradiation, are applied to promote in situ growth of metal halides within the glass substrate. This technique allows the metal halide to be seamlessly encapsulated in the glass matrix, improving the stability of the material. Thus, the metal halide/glass composite is better able to withstand thermal stresses and other environmental factors. Sun et al by modulating CsCd x Pb 1- x Br 3 Middle Cd 2+ And Pb 2+ The ion ratio, which allows tuning of the emission wavelength in the range 461-520nm, shows remarkable stability in ultraviolet and ethanol solvents (Laser Photonics Rev.,2023,2200902). Chen et al successfully prepared CsPbBr with adjustable emission wavelength, high photoluminescence quantum efficiency and good stability 3 Glass and CsPbBr 1.5 I 1.5 The highest photoluminescence quantum efficiency of the glass can reach 94% and 78%, respectively, and after 50 days under the conditions of 85 ℃ and relative humidity of 85%, the PL intensity keeps 94.5% and 92.6% of the initial value (adv. Function. Mater.33,2023, 2213442). However, the crystallization behavior in glass is random. The metal halide producedThe composition, size, distribution and location of the carbide particles are random. Defects in the particle distribution, metal halide/glass interface and glass interior seriously affect the luminescent properties of the material by increasing light scattering and reflection. The combined effect of these factors results in a metal halide/glass composite that has a lower luminous efficiency than a pure metal halide.
In the past decade, copper halide fluorescent materials have received great attention due to their non-toxic, economical, easy to prepare and diversified structural properties. The copper halide material specifically includes CsCu 2 X 3 、Cs 3 Cu 2 X 5 (x=cl, br, I) and a 2 CuX 3 Materials such as (a=k, rb, x=cl, br) have potential applications in solar cells, solid state lighting, X-ray imaging, and lithography fields. Because of the relatively poor thermal stability of copper halide material systems, compounding metal halides with glass systems is an effective method to improve their stability in order to expand the potential for commercial applications. At present, the composite preparation of copper halide and glass material has little research, and the difficulty is mainly that the raw materials CuX (X=Cl, br and I) are not stable in air, so that a more severe preparation process is required to prevent Cu + And (5) oxidizing. Furthermore, the preparation of copper halides into glass substrates under high temperature conditions is a key challenge facing the present study. In order to successfully embed copper halides into glass substrates, a number of factors, such as atmospheric and humidity environmental conditions, must be carefully controlled, as well as the appropriate choice of glass materials. This includes the need to prevent oxidation and degradation of copper halides during the manufacturing process, as this may lead to the formation of impurities, thereby negatively affecting the optical properties of the material.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method and application of a copper halide glass fluorescent material, which can effectively embed copper halide into a glass matrix.
The preparation method of the copper halide glass fluorescent material is characterized by comprising the following steps of:
step 1: fully mixing copper halide with glass matrix, and sealing in a vacuum quartz tube;
step 2: melting and quenching the mixed material in the step 1 through vacuum high-temperature melting;
step 3: and rapidly annealing the molten glass liquid to form the fluorescent material of copper halide and glass.
Further, the copper halides of the present invention include CuX, csCu 2 X 3 、Cs 3 Cu 2 X 5 Wherein x=cl, br, I; or A 2 CuX 3 Wherein a=k, rb, x=cl, br.
Further, the glass substrate comprises one or more of oxide glass and fluoride glass; the oxide glass comprises silicate glass, borate glass and phosphate glass, and the fluoride glass comprises fluoberyllium glass, fluoaluminate glass and fluozirconate glass.
Furthermore, the invention utilizes a grinding and ball milling method to fully mix the copper halide with the glass matrix, wherein the copper halide accounts for 1-15% of the total mass ratio.
Further, the weighing and mixing of the copper halide and the glass substrate according to the present invention are carried out in an inert gas or vacuum atmosphere.
Further, the invention puts copper halide and glass substrate into quartz glass tube to vacuumize and seal.
Further, the glass of the invention has a melting temperature of 600-900 ℃ and a melting time of 5-30 minutes.
Furthermore, the annealing temperature of the glass liquid is 100-250 ℃, and the annealing time is 20-300 minutes.
Further, the prepared copper halide glass material is subjected to cutting, polishing or crushing treatment to obtain copper halide glass blocks with regular shapes or copper halide glass powder with uniform particles.
The copper halide glass fluorescent material is applied to the fields of LED lighting devices, LED display devices, X-ray imaging, anti-counterfeiting and photoetching.
The invention controls the environment of the whole preparation system in a vacuum closed environment to prevent the water absorption and oxidative deterioration of the halide raw material, so that the halide can be directly coated in the glass matrix, and the copper halide fluorescent powder can be directly synthesized in the subsequent heat treatment stage. The preparation method of the invention has simple operation, low cost and good repeatability, and most importantly, avoids Cu + Oxidative deterioration under high temperature conditions. The finally formed copper halide glass composite material has potential application in the fields of LED lighting devices, LED display devices, X-ray imaging, anti-counterfeiting, photoetching and the like.
Drawings
FIG. 1 is a graph showing excitation and luminescence spectra of the CuCl glass composite system prepared in example 1.
FIG. 2 is an XRD pattern of the CuCl glass composite system prepared in example 3.
FIG. 3 is a graph showing excitation and luminescence spectra of CsCl and CuCl glass composite systems prepared in example 7.
Detailed Description
The invention will be described in detail with reference to specific examples. It is to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific qualities, temperatures, times, etc. described below are also merely one example of suitable ranges, i.e., a person skilled in the art may select from the description herein without being limited to the specific values described below.
Firstly, fully mixing copper halide with glass raw materials, sealing the mixture in a vacuum quartz tube, carrying out melting-quenching treatment by vacuum high-temperature melting, and then annealing to form the composite material of the copper halide and the glass. The method has simple operation, low cost, good repeatability, and most importantly, avoids Cu + Oxidative deterioration of (a).
The copper halide is thoroughly mixed with the glass raw material in an inert atmosphere, and the raw material can be uniformly mixed and dispersed by means of mortar grinding or ball milling if necessary.
Wherein the copper halide comprises CuX, csCu 2 X 3 、Cs 3 Cu 2 X 5 (X=Cl, br, I) or A 2 CuX 3 (a=k, rb, x=cl, br). The glass substrate comprises one or more of oxide glass (silicate glass, borate glass, phosphate glass), fluoride glass (fluoberyllium glass, fluoroaluminate glass and fluozirconate glass). The copper halide accounts for not more than 15% of the total mass.
Then, the mixed raw materials are sealed in a vacuum glass tube to create a vacuum environment, and Cu is added + Isolated from oxygen and water.
The vacuum system is placed at high temperature to allow the material to fully form a melt. The melting temperature is 600-900 ℃, preferably 750-800 ℃. The melting hold time is 5 to 30 minutes, preferably 10 to 15 minutes.
The completely melted system is rapidly annealed. The annealing temperature is 100-250 ℃, preferably 150-200 ℃. The annealing time is 20 to 300 minutes, preferably 30 to 90 minutes.
When the system is cooled to room temperature, the luminescence performance of the material is tested. Wherein, the CuCl/boron oxide glass system integrally shows two color luminescence characteristics, one is white light and the other is yellow light, and two luminescence peaks can be found by testing photoluminescence spectra of the CuCl/boron oxide glass system: one in the 440nm blue range and the other in the 550-560nm yellow range; the CsCl and CuCl glass system overall shows green light luminescence characteristics of about 500 nm.
Comparative example 1
CsCl and CuCl are weighed according to the molar ratio of 3:2 in inert atmosphere, raw materials are uniformly mixed through grinding, the mixture is sealed into a quartz tube, and the system is vacuumized;
the system was heated at 400℃for 4 hours by the melt-quenching method to give pure Cs which emit green light at 520nm under excitation light at 320nm 3 Cu 2 Cl 5 Fluorescent powder.
Comparative example 2
Weighing CsBr and CuBr according to a molar ratio of 3:2 in an inert atmosphere, uniformly mixing the raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
the system was heated at 400℃for 12 hours by the melt-quench method to give pure Cs which emitted 454nm blue light at 298nm 3 Cu 2 Br 5 Fluorescent powder.
Comparative example 3
Weighing CsI and CuI according to a molar ratio of 1:2 in an inert atmosphere, uniformly mixing raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
by melt-quenching, the system was heated at 410℃for 10 hours to give pure CsCu which emitted 576nm yellow light under 334nm excitation light 2 I 3 Fluorescent powder.
Example 1
Firstly, weighing CuCl and boron oxide according to the mass ratio of 1:99 in inert atmosphere, uniformly mixing raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 800 ℃ for 10 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 200 ℃ for annealing treatment for 1 hour to obtain the luminescent material composite system with ultraviolet excitation luminescence property. FIG. 1 is a photoluminescence spectrum of a CuCl glass composite system, "lambda ex "and" lambda em "the excitation peak wavelength and the emission peak wavelength, respectively, are the optimum excitation wavelength of 255nm, and there is one luminescence peak at 440nm and 550nm, respectively.
Example 2
Firstly, weighing CuCl and boron oxide according to the mass ratio of 2:98 in inert atmosphere, uniformly mixing raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 850 ℃ for 5 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 150 ℃ for annealing treatment for 1 hour to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
Example 3
Firstly, weighing CuCl and boron oxide according to the mass ratio of 5:95 in an inert atmosphere, uniformly mixing raw materials by a ball milling method, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 750 ℃ for 15 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 250 ℃ for annealing treatment for 30 minutes to obtain the luminescent material composite system with ultraviolet excitation luminescence property. FIG. 2 is an XRD pattern of a CuCl glass composite system, from which it can be seen that there are distinct diffraction peaks of CuCl at diffraction angles of 28.5 °, 47.4 °, 56.3 °, corresponding to (111), (220) and (311) planes of CuCl, respectively, while B can be observed 2 O 3 Diffraction peaks of the (310) crystal plane at a diffraction angle of 27.8 °.
Example 4
Firstly, weighing CuCl and boron oxide according to the mass ratio of 10:90 in an inert atmosphere, uniformly mixing raw materials by a ball milling method, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 700 ℃ for 10 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 100 ℃ for annealing treatment for 1.5 hours to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
Example 5
Firstly, weighing cuprous bromide and boron oxide according to the mass ratio of 1:99 in inert atmosphere, uniformly mixing raw materials by a ball milling method, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 650 ℃ for 15 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 150 ℃ for annealing treatment for 2 hours to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
Example 6
Firstly, weighing copper bromide and boron oxide according to the mass ratio of 5:95 in inert atmosphere, uniformly mixing raw materials through grinding, sealing into a quartz tube, and vacuumizing a system;
secondly, melting the system at 800 ℃ for 10 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 200 ℃ for annealing treatment for 1 hour to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
Example 7
Firstly, weighing CsCl, cuCl and boron oxide according to the mass ratio of 3:1:96 in inert atmosphere, uniformly mixing raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 850 ℃ for 5 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 150 ℃ for annealing treatment for 1 hour to obtain the luminescent material composite system with ultraviolet excitation luminescence property. FIG. 3 shows photoluminescence spectra of CsCl and CuCl glass composite systems, and shows that the optimal excitation wavelength of the luminescent material is 252nm, and a luminescent peak is at 500 nm.
Example 8
Firstly, weighing CsCl, cuCl and boron oxide according to the mass ratio of 3:2:95 in an inert atmosphere, uniformly mixing the raw materials by a ball milling method, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 750 ℃ for 15 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 250 ℃ for annealing treatment for 30 minutes to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
Example 9
Firstly, weighing CsCl, cuCl and boron oxide according to the mass ratio of 4:2:94 in an inert atmosphere, uniformly mixing the raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 700 ℃ for 10 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 100 ℃ for annealing treatment for 1.5 hours to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
Example 10
Firstly, weighing CsCl, cuCl and boron oxide according to the mass ratio of 4:1:95 in an inert atmosphere, uniformly mixing raw materials through grinding, sealing into a quartz tube, and vacuumizing the system;
secondly, melting the system at 650 ℃ for 15 minutes by a melting-quenching method;
and finally, rapidly placing the mixture in an environment of 150 ℃ for annealing treatment for 2 hours to obtain the luminescent material composite system with ultraviolet excitation luminescence property.
The copper halide glass fluorescent material obtained by the preparation method is applied to the fields of LED lighting devices, LED display devices, X-ray imaging, anti-counterfeiting and photoetching.
While the foregoing description of the embodiments of the present invention has been presented in conjunction with the drawings, it should be understood that it is not intended to limit the scope of the invention, but rather, it is intended to cover all modifications or variations within the scope of the invention as defined by the claims of the present invention.

Claims (10)

1. The preparation method of the copper halide glass fluorescent material is characterized by comprising the following steps of:
step 1: fully mixing copper halide with glass matrix, and sealing in a vacuum quartz tube;
step 2: melting and quenching the mixed material in the step 1 through vacuum high-temperature melting;
step 3: and rapidly annealing the molten glass liquid to form the fluorescent material of copper halide and glass.
2. The method for preparing a copper halide glass fluorescent material as claimed in claim 1, wherein the copper halide comprises CuX, csCu 2 X 3 、Cs 3 Cu 2 X 5 Wherein x=cl, br, I; or A 2 CuX 3 One or more of themWherein a=k, rb, x=cl, br.
3. The method for producing a copper halide glass fluorescent material according to claim 1, wherein the glass substrate comprises one or more of oxide glass and fluoride glass; the oxide glass comprises silicate glass, borate glass and phosphate glass, and the fluoride glass comprises fluoberyllium glass, fluoaluminate glass and fluozirconate glass.
4. The method for preparing a copper halide glass fluorescent material according to claim 1, wherein the copper halide is fully mixed with the glass substrate by grinding and ball milling, and the copper halide accounts for 1-15% of the total mass ratio.
5. The method for producing a copper halide glass fluorescent material as claimed in claim 1, wherein the weighing and mixing of the copper halide and the glass substrate are carried out in an inert gas or vacuum atmosphere.
6. The method for producing a copper halide glass fluorescent material as claimed in claim 1, wherein the copper halide glass fluorescent material and the glass substrate are placed in a quartz glass tube, evacuated and sealed.
7. The method for producing a copper halide glass fluorescent material as claimed in claim 1, wherein the glass melting temperature is 600 to 900 ℃ and the melting time is 5 to 30 minutes.
8. The method for preparing a copper halide glass fluorescent material as claimed in claim 1, wherein the glass liquid is annealed at a temperature of 100-250 ℃ for 20-300 minutes.
9. The method for preparing a copper halide glass fluorescent material according to claim 1, wherein the prepared copper halide glass material is subjected to cutting, polishing or crushing treatment to obtain copper halide glass blocks with regular shapes or copper halide glass powder with uniform particles.
10. The application of the copper halide glass fluorescent material is characterized in that the copper halide glass fluorescent material obtained by the preparation method of any one of claims 1-9 is applied to the fields of LED lighting devices, LED display devices, X-ray imaging, anti-counterfeiting and photoetching.
CN202310670482.0A 2023-06-07 2023-06-07 Preparation method and application of copper halide glass fluorescent material Pending CN116693205A (en)

Priority Applications (1)

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CN202310670482.0A CN116693205A (en) 2023-06-07 2023-06-07 Preparation method and application of copper halide glass fluorescent material

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Application Number Priority Date Filing Date Title
CN202310670482.0A CN116693205A (en) 2023-06-07 2023-06-07 Preparation method and application of copper halide glass fluorescent material

Publications (1)

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CN116693205A true CN116693205A (en) 2023-09-05

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