Transparent microcrystalline glass, preparation method and application thereof

By preparing transparent microcrystalline glass with a spotty crystal morphology to replace organic resin, the problems of phosphor aging and decreased luminous efficiency at high temperatures are solved, and an efficient and stable white light source is achieved, which is particularly suitable for outdoor displays and high-power lighting.

CN119118515BActive Publication Date: 2025-10-21WUYI UNIV
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Patent Information

Application Number
CN202411106068.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-13
Publication Date
2025-10-21
Estimated Expiration
2044-08-13

AI Technical Summary

Technical Problem

In existing white light emitting diodes and white light laser diodes, phosphors are easily quenched under long-term high-temperature environments, resulting in decreased luminous efficiency, aging and yellowing of organic resins, and affecting device stability and color rendering.

Method used

Transparent microcrystalline glass is used instead of organic resin. By melting specific components at high temperature and controlling crystallization, α-Sr2SiO4:Eu2+, β-Sr2SiO4:Eu2+ single crystal phase or double crystal phase transparent microcrystalline glass with spotty crystal morphology is prepared, which has excellent stability and luminescence performance.

Benefits of technology

The device's radiation resistance and thermal stability are improved, its service life is extended, and its luminous efficiency is increased to over 74%, making it suitable for display and high-power lighting fields.

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Abstract

The application belongs to the technical field of solid light-emitting materials, and discloses a transparent microcrystalline glass as well as a preparation method and application thereof. 2+ The transparent microcrystalline glass comprises α-Sr2SiO4:Eu 2+ The transparent microcrystalline glass comprises α-Sr2SiO4:Eu 2+ The transparent microcrystalline glass comprises α-Sr2SiO4:Eu 2+ The transparent microcrystalline glass comprises α-Sr2SiO4:Eu The transparent microcrystalline glass has excellent stability and light-emitting performance, and can be widely applied to the fields of display or illumination, and is particularly suitable for the fields of outdoor display and high-power illumination.
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Description

Technical Field

[0001] The present invention belongs to the technical field of solid luminescent materials, and in particular relates to a transparent microcrystalline glass and a preparation method and application thereof. Background Art

[0002] Solid-state lighting technology is developing towards higher brightness, lower power consumption, smaller size, and lower cost. White light-emitting diodes (WLEDs) and white laser diodes (WLDs) have attracted widespread market attention in recent years due to their high efficiency, high brightness, long life, and environmental friendliness.

[0003] At present, there are generally three solutions to achieve white light sources. The first solution is to combine three separate monochromatic LED / LD (light emitting diode / laser diode) chips to emit red, green and blue light to obtain white light. This method has a wide color gamut and high luminous efficiency. The second solution is to combine a blue LED / LD chip with a yttrium aluminum garnet YAG:Ce 3+ WLEDs / WLDs, made with yellow phosphor, have captured over half of the white light market due to their high luminous efficiency and low cost. A third approach combines 365nm UV LEDs / LDs with UV-excited red, green, and blue phosphors. This WLED approach offers advantages in color uniformity and high color rendering.

[0004] Due to the high cost of chips, the solution of combining red, green and blue chips to obtain white light is not recognized by the public, so the most widely used WLED / WLD on the market is mainly made by using LED / LD chips as a substrate and adding corresponding phosphors. Generally speaking, white light sources are generally obtained by irradiating LED / LD chips on phosphors that are fully mixed with organic resins for light conversion. Under such long-term irradiation in high-temperature environments, phosphors will face problems such as thermal quenching and decreased luminous efficiency. In addition, long-term irradiation will also accelerate the aging and yellowing of organic resins, and even ablation, which will bring serious problems such as color drift and malfunction of lighting devices. In addition, the luminescence performance and stability (such as thermal stability) of existing solid-state luminescent materials also need to be further improved.

[0005] Therefore, in order to solve the above problems, there is an urgent need for an all-inorganic solid luminescent material with excellent optical properties that does not require the use of organic resin for auxiliary packaging and also has good luminescent properties and stability. Summary of the Invention

[0006] The present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art. To this end, the present invention proposes a transparent microcrystalline glass, a preparation method thereof and an application thereof. The transparent microcrystalline glass of the present invention is a fully inorganic fluorescent transparent microcrystalline glass, which has excellent stability and luminescence performance. The use of the transparent microcrystalline glass of the present invention to replace the traditional fluorescent film mixed with organic resin and phosphor covering the LED / LD chip can effectively prevent the decline in luminescence efficiency and the aging, yellowing and carbonization of the organic resin. Therefore, the WLED / WLD device prepared by coupling the transparent microcrystalline glass with the LED / LD chip having good radiation resistance, excellent luminescence efficiency and thermal stability and low manufacturing cost will have the advantages of longer service life and excellent luminescence performance, and can be widely used in the display or lighting field, and is particularly suitable for outdoor display and high-power lighting fields.

[0007] The transparent micro-ceramic glass of the present invention is a fluorescent α-Sr2SiO4:Eu with a spot-like crystal morphology that can be obtained by controlling the crystallization of specific component raw materials at a specific heating and melting temperature. 2+ Single crystal phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, and α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ Dual-crystal phase transparent glass-ceramics. This transparent glass-ceramics exhibits excellent stability (retaining over 70% of its initial luminous intensity at 150°C) and superior luminous performance (quantum efficiency exceeding 74%). It can be widely used in display or lighting applications, and is particularly well-suited for outdoor displays and high-power lighting.

[0008] A first aspect of the present invention provides a transparent glass-ceramic.

[0009] Specifically, a transparent microcrystalline glass includes α-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, or α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ At least one of the twin crystal phases.

[0010] Preferably, the α-Sr2SiO4:Eu 2+ The single crystal phase has a spotty crystal morphology.

[0011] Preferably, the β-Sr2SiO4:Eu 2+ The single crystal phase has a spotty crystal morphology.

[0012] Preferably, the α-Sr2SiO4:Eu2+ and β-Sr2SiO4:Eu 2+ The twin crystal phase has a spotty crystal morphology.

[0013] Preferably, the α-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The grain length of the twin crystal phase is 1-12 μm, more preferably 2-10 μm.

[0014] Preferably, the transparent glass-ceramics can emit a strong broadband spectrum in the 400 to 700 nm band under 365 nm light excitation, and further the main emission peak is located at 532 nm.

[0015] Preferably, the quantum efficiency of the transparent glass-ceramics is not less than 74%, for example, 75-85%.

[0016] Preferably, the transparent glass-ceramics still retains more than 70% of the initial luminous intensity at 150° C. For example, the luminous intensity retains 70-85% of the initial luminous intensity.

[0017] A second aspect of the present invention provides a method for preparing transparent glass-ceramics.

[0018] Specifically, a method for preparing transparent glass-ceramics includes the following steps:

[0019] Weighing SiO2, SrO, and Eu2O3 raw materials, then mixing them, heating and melting them under a reducing atmosphere, and then cooling them to obtain the transparent microcrystalline glass;

[0020] In the raw material, the molar percentage of SiO2 is 40-60%, the molar percentage of SrO is 40-60%, and the molar percentage of SrO is greater than the molar percentage of SiO2;

[0021] The heating and melting temperature exceeds 1510°C.

[0022] Preferably, in the raw material, the molar percentage of Eu2O3 is 0.01-2%, more preferably 0.1-0.5%.

[0023] Preferably, in the raw material, the molar percentage of SiO2 is 40-60%, the molar percentage of SrO is 40-60%, the molar percentage of Eu2O3 is 0.01-2%, and the molar percentage of SrO is greater than the molar percentage of SiO2.

[0024] Further preferably, in the raw materials, the molar percentage of SiO2 is 45%, the molar percentage of SrO is 54.9%, and the molar percentage of Eu2O3 is 0.1%.

[0025] Preferably, the heating and melting temperature is 1570-1640°C, more preferably 1580-1600°C.

[0026] Preferably, the heating and melting temperature is 1570-1640° C. and maintained for 0.8-6 hours, more preferably for 1-2 hours.

[0027] Preferably, the reducing atmosphere is selected from at least one of H2, CO or carbon powder.

[0028] Preferably, the mixing process is performed by grinding, for example, for 20-30 minutes.

[0029] Preferably, the cooling is natural cooling to room temperature, for example, cooling to room temperature in a muffle furnace.

[0030] Preferably, the cooling time is 6-12 hours, more preferably 8-10 hours.

[0031] A third aspect of the present invention provides an application of a transparent glass-ceramic.

[0032] A display or lighting device comprises the transparent micro-ceramic glass.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] (1) The present invention adopts specific preparation conditions (raw material ratio and heating melting temperature) to prepare transparent fluorescent α-Sr2SiO4:Eu with spot-like crystal morphology. 2+ Single crystal phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, or α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The bicrystalline transparent glass-ceramic has a hard, dense, and uniform texture and possesses stable physical and chemical properties. Due to its excellent stability (retaining over 70% of its initial luminous intensity at 150°C) and superior luminous performance (quantum efficiency exceeding 74%), it can be widely used in display and lighting applications, particularly outdoor displays and high-power lighting.

[0035] (2) α-Sr2SiO4:Eu under ultraviolet light excitation 2+ Single crystal phase transparent glass-ceramics, α-Sr2SiO4:Eu 2+Single crystal phase and β-Sr2SiO4:Eu 2+ Double crystal phase transparent glass-ceramics can emit strong green light (quantum efficiency reaches 75%), β-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics can emit yellow-green light.

[0036] (3) The present invention prepares a phase-changeable transparent fluorescent microcrystalline glass containing a spot-like crystal morphology. The crystal phase in the microcrystalline glass can be changed from α-Sr2SiO4:Eu 2+ Single-phase modulation α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ Twin phase, then β-Sr2SiO4:Eu 2+ Single phase.

[0037] (4) The transparent microcrystalline glass of the present invention is prepared in a one-step process, which has simple process, low cost, non-toxicity and pollution-free. The transparent microcrystalline glass material has excellent luminescence performance and can be developed as a green broadband fluorescent solid luminescent material and applied in solid-state lighting. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 This is the XRD pattern of the precursor amorphous glass of Comparative Example 1 of the present invention;

[0039] Figure 2 This is a digital photo of the precursor amorphous glass of Comparative Example 1 of the present invention;

[0040] Figure 3 The normalized excitation and emission spectra of the precursor amorphous glass of Comparative Example 1 of the present invention are shown;

[0041] Figure 4 This is the XRD pattern of the transparent glass-ceramics of Example 1 of the present invention;

[0042] Figure 5 This is a digital photo of the transparent glass-ceramics of Example 1 of the present invention;

[0043] Figure 6 This is a morphology image of the transparent glass-ceramics of Example 1 of the present invention taken under a scanning electron microscope (SEM);

[0044] Figure 7 Graphs showing the normalized excitation and emission spectra of the transparent glass-ceramics of Example 1 of the present invention;

[0045] Figure 8 This is a morphology image taken by a scanning electron microscope (SEM) of the transparent glass-ceramics in Example 2 of the present invention;

[0046] Figure 9 Graphs showing the normalized excitation and emission spectra of the transparent glass-ceramics of Example 2 of the present invention;

[0047] Figure 10 This is a temperature-varying spectrum diagram of the transparent glass-ceramics of Example 2 of the present invention;

[0048] Figure 11 Graphs showing the normalized excitation and emission spectra of the transparent glass-ceramics of Example 3 of the present invention;

[0049] Figure 12 This is a morphology image taken by a scanning electron microscope (SEM) of the transparent glass-ceramics in Example 4 of the present invention;

[0050] Figure 13 These are the normalized excitation and emission spectra of the transparent glass-ceramics of Example 4 of the present invention.

[0051] Figure 14 This is the XRD pattern of the amorphous glass of Comparative Example 3 of the present invention. DETAILED DESCRIPTION

[0052] In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the following examples are given for illustration. It should be noted that the following examples do not limit the scope of protection claimed by the present invention.

[0053] Unless otherwise specified, the raw materials, reagents, or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.

[0054] Figure 1 、 Figure 4 、 Figure 14 "Intensity" means intensity, 2θ means diffraction angle, and "degree" means degree. Figure 4 The “PDF#39-1256” in the table indicates the standard card for β-Sr2SiO4, and the “PDF#38-0271” indicates the standard card for α-Sr2SiO4.

[0055] Figure 3 、 Figure 7 、 Figure 9 、 Figure 11 、 Figure 13 "Intensity" here means intensity, and "Wavelength" means wavelength.

[0056] Figure 10 "Wavelength" here means wavelength, "Temperature" means temperature, "High" means high, and "Low" means low.

[0057] Comparative Example 1

[0058] A method for preparing a precursor amorphous glass comprises the following steps:

[0059] S1. Weigh the required raw materials SiO2, SrO, and Eu2O3 according to the molar fractions of 45 mol% SiO2, 54.9 mol% SrO, and 0.1 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials into a crucible;

[0060] S2. Place the crucible containing the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, and keep it warm in a muffle furnace at 1600°C for 1 hour to melt it. Take it out immediately after melting, and pour the melt into a copper mold preheated at 500°C to obtain the precursor amorphous glass.

[0061] from Figure 1 It can be seen from the X-ray diffraction peaks that there is no crystal diffraction peak in the precursor amorphous glass prepared in this comparative example 1, indicating that amorphous glass is prepared.

[0062] The precursor amorphous glass prepared in this comparative example 1 still has excellent transparency when the thickness is 3 mm (see Figure 2 , you can see the word "Glass").

[0063] Under the excitation of 365nm wavelength violet light, the precursor amorphous glass prepared in this comparative example 1 exhibits bright yellow luminescence. The normalized excitation and emission spectra at room temperature are measured using an Edinburgh FS980 fluorescence spectrometer. Figure 3 As shown; the emission spectrum can be observed Eu 2+ 4f of ions 6 5d 1 -4f 7 transitions, which are typically broad-peak emissions, but there are also some corresponding to Eu 3+ Its luminescence center wavelength is at 588nm, the excitation spectrum covers a wide band of 250n-500nm, and the excitation peak is at 400nm.

[0064] Comparative Example 2

[0065] A method for preparing glass, comprising the following steps:

[0066] S1. Weigh the required raw materials SiO2, SrO, and Eu2O3 according to the molar fractions of 45 mol% SiO2, 54.9 mol% SrO, and 0.1 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials into a crucible;

[0067] S2. Place the crucible containing the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, keep the crucible at 1400°C in a muffle furnace for 1 hour, and then slowly cool the crucible from 1400°C to room temperature over 8 hours to obtain the product.

[0068] In this comparative example, due to the low melting temperature, bulk glass-ceramics cannot be obtained.

[0069] Comparative Example 3

[0070] A method for preparing amorphous glass comprises the following steps:

[0071] S1. Weigh the required raw materials SiO2, BaO, and Eu2O3 according to the molar fractions of 70 mol% SiO2, 29.5 mol% SrO, and 0.5 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials in a crucible;

[0072] S2. Place the crucible containing the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, keep it warm in a muffle furnace at 1600°C for 1 hour to melt it, and then slowly cool it from 1600°C to room temperature in the muffle furnace over 8 hours to obtain a block of amorphous glass.

[0073] The XRD pattern of the amorphous glass prepared in this comparative example is shown in FIG. Figure 14 As shown. Figure 14 It can be seen from the X-ray diffraction peaks that there is no crystal diffraction peak in the amorphous glass prepared in this comparative example, indicating that amorphous glass is prepared.

[0074] Example 1

[0075] A transparent microcrystalline glass comprising α-Sr2SiO4:Eu 2+ Single crystal phase.

[0076] A method for preparing transparent glass-ceramics comprises the following steps:

[0077] S1. Weigh the required raw materials SiO2, SrO, and Eu2O3 according to the molar fractions of 45 mol% SiO2, 54.99 mol% SrO, and 0.01 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials into a crucible;

[0078] S2. Place the crucible with the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, keep it in a muffle furnace at 1600℃ for 1 hour to melt it, and then slowly cool it from 1600℃ to room temperature over 8 hours to obtain a block of α-Sr2SiO4:Eu 2+ Transparent glass-ceramics in a single crystal phase.

[0079] from Figure 4 It can be seen from the X-ray diffraction peak that α-Sr2SiO4:Eu has been precipitated in the transparent micro-ceramic glass prepared in this embodiment. 2+ Single crystal phase.

[0080] The transparent glass-ceramics prepared in this embodiment still has a certain degree of transparency when the thickness is 2 mm (see Figure 5 (a) in the figure), it was further observed under a scanning electron microscope (SEM) that a microcrystalline glass with a 2-10 μm spot-like crystal morphology was successfully prepared (see Figure 6 ).

[0081] Under the excitation of 365nm wavelength violet light, the transparent micro-ceramic glass prepared in this embodiment exhibits bright green luminescence. The normalized excitation and emission spectra at room temperature are measured using an Edinburgh FS980 fluorescence spectrometer. Figure 7 As shown; the emission spectrum can be observed Eu 2+ 4f of ions 6 5d 1 -4f 7 The transition is a typical broad-peak emission with a central wavelength of 532 nm. The excitation spectrum covers a wide band of 250-450 nm, and the excitation peak is at 365 nm.

[0082] Example 2

[0083] A transparent microcrystalline glass comprising α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ Twin crystal phase.

[0084] A method for preparing transparent glass-ceramics comprises the following steps:

[0085] S1. Weigh the required raw materials SiO2, SrO, and Eu2O3 according to the molar fractions of 45 mol% SiO2, 54.9 mol% SrO, and 0.1 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials into a crucible;

[0086] S2. Place the crucible with the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, keep it in a muffle furnace at 1600℃ for 1 hour to melt it, and then slowly cool it from 1600℃ to room temperature over 8 hours to obtain a block of α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ Transparent glass-ceramics with twin crystal phases.

[0087] from Figure 4 It can be seen from the X-ray diffraction peak that α-Sr2SiO4:Eu has been precipitated in the transparent micro-ceramic glass prepared in this embodiment. 2+ and β-Sr2SiO4:Eu 2+ Twin crystal phase.

[0088] The transparent glass-ceramics prepared in this embodiment still has a certain degree of transparency when the thickness is 2 mm (see Figure 5 (b) in the figure), it was further observed under a scanning electron microscope (SEM) that a microcrystalline glass with a 2-10 μm spot-like crystal morphology was successfully prepared (see Figure 8 ).

[0089] Under the excitation of 365nm wavelength violet light, the transparent micro-ceramic glass prepared in this embodiment exhibits bright green luminescence. The normalized excitation and emission spectra at room temperature are measured using an Edinburgh FS980 fluorescence spectrometer. Figure 9 As shown; the emission spectrum can be observed Eu 2+ 4f of ions 6 5d 1 -4f 7 The transition is a typical broad-peak emission with a central wavelength of 532 nm. The excitation spectrum covers a wide band of 250-450 nm, and the excitation peak is at 365 nm.

[0090] Figure 10 This is the temperature-varying spectrum of the transparent microcrystalline glass of Example 2 at 300K-520K. It can be seen intuitively that the transparent microcrystalline glass still retains 70% of the initial luminous intensity at 423.15K, further verifying that the transparent fluorescent microcrystalline glass of the present invention has good thermal stability.

[0091] Example 3

[0092] A transparent microcrystalline glass comprising α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ Twin crystal phase.

[0093] A method for preparing transparent glass-ceramics comprises the following steps:

[0094] S1. Weigh the required raw materials SiO2, SrO, and Eu2O3 according to the molar fractions of 45 mol% SiO2, 54.6 mol% SrO, and 0.4 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials into a crucible;

[0095] S2. Place the crucible with the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, keep it in a muffle furnace at 1600℃ for 1 hour to melt it, and then slowly cool it from 1600℃ to room temperature over 8 hours to obtain a block of α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ Transparent glass-ceramics with twin crystal phases.

[0096] from Figure 4It can be seen from the X-ray diffraction peak that α-Sr2SiO4:Eu has been precipitated in the transparent micro-ceramic glass prepared in this embodiment. 2+ and β-Sr2SiO4:Eu 2+ Twin crystal phase.

[0097] Under the excitation of 365nm wavelength violet light, the transparent micro-ceramic glass prepared in this embodiment exhibits bright green luminescence. The normalized excitation and emission spectra at room temperature are measured using an Edinburgh FS980 fluorescence spectrometer. Figure 11 As shown; the emission spectrum can be observed Eu 2+ 4f of ions 6 5d 1 -4f 7 The transition is a typical broad-peak emission with a central wavelength of 532 nm. The excitation spectrum covers a wide band of 250-450 nm, and the excitation peak is at 365 nm.

[0098] Example 4

[0099] A transparent microcrystalline glass comprising β-Sr2SiO4:Eu 2+ Single crystal phase.

[0100] A method for preparing transparent glass-ceramics comprises the following steps:

[0101] S1. Weigh the required raw materials SiO2, SrO, and Eu2O3 according to the molar fractions of 45 mol% SiO2, 54.3 mol% SrO, and 0.7 mol% Eu2O3, mix and grind them for 30 minutes, and place the mixed and ground raw materials into a crucible;

[0102] S2. Place the crucible with the raw materials in a large crucible with a lid covered with activated carbon powder as a reducing atmosphere, keep it in a muffle furnace at 1600℃ for 1 hour to melt it, and then slowly cool it from 1600℃ to room temperature over 8 hours to obtain a block of β-Sr2SiO4:Eu 2+ Transparent glass-ceramics in a single crystal phase.

[0103] from Figure 4 It can be seen from the X-ray diffraction peak that β-Sr2SiO4:Eu has been precipitated in the transparent glass-ceramics prepared in this embodiment. 2+ Single crystal phase.

[0104] The transparent glass-ceramics prepared in this embodiment still has a certain degree of transparency when the thickness is 2 mm (see Figure 5 (c)), it was further observed under a scanning electron microscope (SEM) that a microcrystalline glass with a 2-10 μm spot-like crystal morphology was successfully prepared (see Figure 12 ).

[0105] Under the excitation of violet light with a wavelength of 365 nm, the transparent micro-ceramic glass prepared in this embodiment exhibits bright yellow-green luminescence. The normalized excitation and emission spectra at room temperature are measured using an Edinburgh FS980 fluorescence spectrometer. Figure 13 As shown; the emission spectrum can be observed Eu 2+ 4f of ions 6 5d 1 -4f 7 The transition is a typical broad-peak emission with a central wavelength of 500 nm. The excitation spectrum covers a wide band of 250-450 nm, and the excitation peak is at 325 nm.

[0106] A display device includes the transparent microcrystalline glass of embodiment 1.

[0107] A lighting device comprises the transparent microcrystalline glass of embodiment 2.

[0108] On the basis of the above embodiments and within the scope of protection requested by the present invention, changes to the technical solutions of the present invention, such as changes in the amount of raw materials of the present invention, temperature and time, etc., which do not require creative labor, all fall within the scope of protection of the present invention.

Claims

1. A transparent glass-ceramic, characterized in that: Including α-Sr2SiO4:Eu 2+ Single crystal phase, β-Sr2SiO4:Eu 2+ Single crystal phase, or α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ at least one of the twin crystal phases; The α-Sr2SiO4:Eu 2+ The single crystal phase has a spot-like crystal morphology, and the β-Sr2SiO4:Eu 2+ The single crystal phase has a spot-like crystal morphology, and the α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The twin crystal phase has a spotty crystal morphology.

2. The transparent glass-ceramics according to claim 1, characterized in that: The α-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ Single crystal phase transparent glass-ceramics, α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The grain length of the twin crystal phase is 1-12 μm.

3. The transparent glass-ceramics according to claim 1, characterized in that: The transparent microcrystalline glass can emit a broadband spectrum in the 400 to 700 nm band under 365 nm light excitation.

4. The transparent glass-ceramics according to claim 1, characterized in that: The quantum efficiency of the transparent microcrystalline glass is not less than 74%.

5. The transparent glass-ceramics according to claim 1, characterized in that: The transparent microcrystalline glass still retains more than 70% of the initial luminous intensity at 150°C.

6. The method for preparing the transparent glass-ceramics according to any one of claims 1 to 5, characterized in that: The following steps are involved: Weighing SiO2, SrO, and Eu2O3 raw materials, then mixing them, heating and melting them under a reducing atmosphere, and then cooling them to obtain the transparent microcrystalline glass; In the raw materials, the molar percentage of SiO2 is 40-60%, the molar percentage of SrO is 40-60%, the molar percentage of SrO is greater than the molar percentage of SiO2, and the sum of the raw material components is 100%; The heating and melting temperature exceeds 1510°C.

7. The preparation method according to claim 6, characterized in that In the raw materials, the molar percentage of Eu2O3 is 0.01-2%.

8. The preparation method according to claim 6, characterized in that The heating and melting temperature is 1570-1640° C., and the heating and melting temperature of 1570-1640° C. is maintained for 0.8-6 hours; and / or, the reducing atmosphere is selected from at least one of H 2 , CO or carbon powder.

9. A display or lighting device, characterized in that: The transparent microcrystalline glass comprises the transparent microcrystalline glass according to any one of claims 1 to 5.

Citation Information

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