Transparent glass-ceramic, and preparation method therefor and use thereof
By preparing transparent microcrystalline glass with a speckled crystal morphology to replace organic resin and phosphor, the problems of decreased luminous efficiency and stability in white LED/LD devices are solved, achieving high efficiency and stable optical performance, suitable for display and high-power lighting.
Patent Information
- Application Number
- PCT/CN2024/113914
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-08-13
- Filing Date
- 2024-08-22
- Publication Date
- 2026-02-19
AI Technical Summary
In existing white LED/LD devices, phosphors are prone to quenching under long-term high-temperature environments, resulting in decreased luminous efficiency. Organic resins age and turn yellow, leading to color drift and device failure. Furthermore, the stability and luminous performance of solid-state light-emitting materials need to be improved.
By replacing the traditional organic resin and phosphor mixture structure with transparent microcrystalline glass, and controlling the crystallization of specific components after high-temperature melting, α-Sr2SiO4:Eu2+ and β-Sr2SiO4:Eu2+ single crystals or bicrystalline phase transparent microcrystalline glasses with speckled crystal morphology are prepared, which have excellent stability and luminescence performance.
It improves the device's radiation resistance and thermal stability, extends its service life, and increases luminous efficiency to over 74%, making it suitable for display and high-power lighting applications.
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Figure CN2024113914_19022026_PF_FP_ABST
Abstract
Description
Transparent microcrystalline glass and preparation method and application thereof TECHNICAL FIELD
[0001] The present application belongs to the technical field of solid-state luminescent materials, and particularly relates to a transparent microcrystalline glass and a preparation method and application thereof. BACKGROUND
[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 light laser diodes (WLDs) have attracted widespread attention in the market in recent years due to their high efficiency, high brightness, long service life and environmental protection.
[0003] Currently, there are generally three schemes to realize white light sources. The first scheme is to combine three separate monochromatic LED / LD (light emitting diode / laser diode) chips to emit red, green and blue light mixed to obtain white light. This method has a wide color gamut and high luminous efficiency. The second scheme is to combine a blue light LED / LD chip with a yellow fluorescent powder YAG:Ce 3+ WLED / WLD made by matching. This white light illuminating device has high luminous efficiency and low cost and has occupied more than half of the white light illuminating market. The third scheme is to combine a 365 nm ultraviolet LED / LD chip with red, green and blue fluorescent powders excited by ultraviolet waves. This WLED has the advantages of good color uniformity and high color rendering.
[0004] Due to the high cost of chips, the scheme of combining red, green and blue chips to obtain white light is not recognized by the public, so the most widely used WLED / WLD in the market is mainly made by adding corresponding fluorescent powders to the LED / LD chip as the substrate. Generally, a white light source is obtained by irradiating a LED / LD chip on a fluorescent powder fully mixed with an organic resin for light conversion. The fluorescent powder will face problems such as thermal quenching and luminous efficiency decline under such long-term high-temperature irradiation. In addition, long-term irradiation will also accelerate the aging and yellowing of the organic resin, and even ablation, which will bring serious problems such as color drift and failure of the illuminating device to work normally. In addition, the luminous performance and stability (such as thermal stability) of the existing solid-state luminescent materials need to be further improved.
[0005] Therefore, in order to solve the above problems, it is urgent to need a full-inorganic solid-state luminescent material with excellent optical performance without the need for auxiliary packaging with an organic resin, and also with good luminous performance and stability.
[0006] SUMMARY
[0007] The present application aims to at least solve one of the technical problems existing in the prior art. To this end, the present application proposes a transparent microcrystalline glass as well as a preparation method and application thereof. The transparent microcrystalline glass according to the present application belongs to a kind of all-inorganic fluorescent transparent microcrystalline glass, has excellent stability and luminescence performance, and can effectively prevent the phenomena of luminescent efficiency reduction, aging, yellowing and carbonization of organic resin by using the transparent microcrystalline glass according to the present application to replace the conventional fluorescent film mixed with organic resin and fluorescent powder on the LED / LD chip. Therefore, the WLED / WLD device prepared by coupling the LED / LD chip with the transparent microcrystalline glass according to the present application which has good anti-radiation performance, excellent luminescent efficiency and thermal stability and low manufacturing cost will have a longer service life and excellent luminescent performance, and can be widely applied in display or lighting fields, and is particularly suitable for outdoor display and high-power lighting fields.
[0008] The transparent microcrystalline glass according to the present application is a fluorescent α-Sr2SiO4:Eu 2+ single-crystal phase transparent microcrystalline glass, β-Sr2SiO4:Eu 2+ single-crystal phase transparent microcrystalline glass, and α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double-crystal phase transparent microcrystalline glass. The transparent microcrystalline glass has excellent stability (retains more than 70% of the initial luminescent intensity at 150℃) and excellent luminescent performance (quantum efficiency is more than 74%), and can be widely applied in display or lighting fields, and is particularly suitable for outdoor display and high-power lighting fields.
[0009] The first aspect of the present application provides a transparent microcrystalline glass.
[0010] Specifically, a transparent microcrystalline glass comprises α-Sr2SiO4:Eu 2+ single-crystal phase transparent microcrystalline glass, β-Sr2SiO4:Eu 2+ single-crystal phase transparent microcrystalline glass, or α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ at least one of double-crystal phases.
[0011] Preferably, the α-Sr2SiO4:Eu 2+ single-crystal phase has a spot-like crystal morphology.
[0012] Preferably, the β-Sr2SiO4:Eu 2+ single-crystal phase has a spot-like crystal morphology.
[0013] Preferably, the α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The double crystal phase has a spot-like crystal morphology.
[0014] Preferably, the α-Sr2SiO4:Eu 2+ The single crystal phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ The single crystal phase transparent glass-ceramics, α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The grain length of the double crystal phase is 1-12 μm, and is further preferably 2-10 μm.
[0015] Preferably, the transparent glass-ceramics can emit a strong broadband spectrum in the 400-700 nm wavelength range under 365 nm light excitation, and the main emission peak is further at 532 nm.
[0016] Preferably, the quantum efficiency of the transparent glass-ceramics is not less than 74%, for example, 75-85%.
[0017] Preferably, the transparent glass-ceramics still retains more than 70% of the initial luminescence intensity at 150°C. For example, the luminescence intensity retains 70-85% of the initial luminescence intensity.
[0018] The second aspect of the present application provides a preparation method of the transparent glass-ceramics.
[0019] Specifically, the preparation method of the transparent glass-ceramics comprises the following steps:
[0020] The SiO2, SrO and Eu2O3 raw materials are weighed and then mixed, and then melted under a reducing atmosphere, and then cooled to obtain the transparent glass-ceramics;
[0021] In the raw materials, the molar percentage of the SiO2 is 40-60%, the molar percentage of the SrO is 40-60%, and the molar percentage of the SrO is greater than the molar percentage of the SiO2;
[0022] The melting temperature is higher than 1510°C.
[0023] Preferably, in the raw materials, the molar percentage of the Eu2O3 is 0.01-2%, and is further preferably 0.1-0.5%.
[0024] Preferably, in the raw materials, the molar percentage of the SiO2 is 40-60%, the molar percentage of the SrO is 40-60%, the molar percentage of the Eu2O3 is 0.01-2%, and the molar percentage of the SrO is greater than the molar percentage of the SiO2.
[0025] Further preferably, in the raw material, the molar percentage of SiO2 is 45%, the molar percentage of SrO is 54.9%, and the molar percentage of Eu2O3 is 0.1%.
[0026] Preferably, the temperature of the heating melting is 1570-1640℃, and further preferably 1580-1600℃.
[0027] Preferably, the temperature of the heating melting is 1570-1640℃, and further preferably 1580-1600℃.
[0028] Preferably, the reducing atmosphere is selected from at least one of H2, CO or carbon powder.
[0029] Preferably, the mixing process is carried out by grinding. For example, grinding for 20-30 minutes.
[0030] Preferably, the cooling is natural cooling to room temperature, for example, cooling to room temperature with a muffle furnace.
[0031] Preferably, the cooling time is 6-12 hours, and further preferably 8-10 hours.
[0032] The third aspect of the present application provides an application of the transparent microcrystalline glass.
[0033] A display or lighting device comprising the transparent microcrystalline glass.
[0034] Compared with the prior art, the present application has the following beneficial effects:
[0035] (1) The present application adopts specific preparation conditions (raw material ratio and heating melting temperature) to prepare the transparent fluorescent α-Sr2SiO4:Eu 2+ monocrystal phase transparent microcrystalline glass, β-Sr2SiO4:Eu 2+ monocrystal phase transparent microcrystalline glass, or α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ bimorph crystal phase transparent microcrystalline glass, which is hard, compact and uniform in texture, and has the characteristics of stable physical and chemical properties. The transparent microcrystalline glass has excellent stability (retains more than 70% of the initial luminescence intensity at 150℃) and excellent luminescence performance (quantum efficiency is more than 74%), and can be widely used in the field of display or lighting, especially in the field of outdoor display and high-power lighting.
[0036] (2) Under ultraviolet excitation, α-Sr2SiO4:Eu 2+ monocrystal phase transparent microcrystalline glass, α-Sr2SiO4:Eu2+ single crystal phase and β-Sr2SiO4:Eu 2+ The double crystal phase transparent glass-ceramics can emit strong green light (quantum efficiency reaches 75%), β-Sr2SiO4:Eu 2+ The single crystal phase transparent glass-ceramics can emit yellow-green light.
[0037] (3) The present application prepares a phase-changeable transparent fluorescent glass-ceramics containing spot-shaped crystal morphology, the crystal phase in the glass-ceramics can change from α-Sr2SiO4:Eu 2+ single phase modulation α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phase, to β-Sr2SiO4:Eu 2+ single phase.
[0038] (4) The transparent glass-ceramics of the present application is prepared by one-step method, the process is simple, the cost is low, non-toxic and non-polluting, the transparent glass-ceramics material has excellent luminescent performance, and can be developed and applied in solid-state lighting as a green broadband fluorescent solid-state luminescent material. BRIEF DESCRIPTION OF DRAWINGS
[0039] Fig. 1 is an XRD diagram of the precursor amorphous glass of the comparative example 1 of the present application;
[0040] Fig. 2 is a digital photograph diagram of the precursor amorphous glass of the comparative example 1 of the present application;
[0041] Fig. 3 is a normalized excitation and emission spectrum diagram of the precursor amorphous glass of the comparative example 1 of the present application;
[0042] Fig. 4 is an XRD diagram of the transparent glass-ceramics of the embodiment 1 of the present application;
[0043] Fig. 5 is a digital photograph diagram of the transparent glass-ceramics of the embodiment 1 of the present application;
[0044] Fig. 6 is a morphology diagram taken by scanning electron microscope (SEM) of the transparent glass-ceramics of the embodiment 1 of the present application;
[0045] Fig. 7 is a normalized excitation and emission spectrum diagram of the transparent glass-ceramics of the embodiment 1 of the present application;
[0046] Fig. 8 is a morphology diagram taken by scanning electron microscope (SEM) of the transparent glass-ceramics of the embodiment 2 of the present application;
[0047] Fig. 9 is a normalized excitation and emission spectrum diagram of the transparent glass-ceramics of the embodiment 2 of the present application;
[0048] Fig. 10 is a variable temperature spectrum diagram of the transparent glass-ceramics of the embodiment 2 of the present application;
[0049] Fig. 11 is a normalized excitation and emission spectrum of the transparent glass-ceramic of Example 3 of the present application;
[0050] Fig. 12 is a scanning electron microscope (SEM) morphology of the transparent glass-ceramic of Example 4 of the present application;
[0051] Fig. 13 is a normalized excitation and emission spectrum of the transparent glass-ceramic of Example 4 of the present application.
[0052] Fig. 14 is an XRD pattern of the amorphous glass of Comparative Example 3 of the present application. DETAILED DESCRIPTION
[0053] In order to make the skilled in the art more clearly understand the technical solutions described in the present application, the following examples are listed for illustration. It should be noted that the following examples do not constitute a limitation on the scope of protection required by the present application.
[0054] The raw materials, reagents or devices used in the following examples, if not specifically stated, can be obtained from conventional commercial channels, or can be obtained by existing known methods.
[0055] In Fig. 1, Fig. 4, Fig. 14, "Intensity" represents intensity, 2θ represents diffraction angle, "degree" represents degree, "PDF # 39-1256" in Fig. 4 represents the standard card of β-Sr2SiO4, and "PDF # 38-0271" represents the standard card of α-Sr2SiO4.
[0056] In Fig. 3, Fig. 7, Fig. 9, Fig. 11, Fig. 13, "Intensity" represents intensity, and "Wavelength" represents wavelength.
[0057] In Fig. 10, "Wavelength" represents wavelength, "Temperature" represents temperature, "High" represents high, and "Low" represents low.
[0058] Comparative Example 1
[0059] A method for preparing a precursor amorphous glass, comprising the following steps:
[0060] S1, according to the molar fractions of 45 mol% SiO2, 54.9 mol% SrO and 0.1 mol% Eu2O3, the required raw materials SiO2, SrO and Eu2O3 are weighed and mixed and ground for 30 min, and the mixed and ground uniform raw materials are placed in a crucible;
[0061] S2. Place the crucible containing the raw material into a large covered crucible filled with activated carbon powder as a reducing atmosphere. Keep it in a muffle furnace at 1600℃ for 1 hour to melt it. Immediately after melting, remove it and pour the melt into a copper mold preheated at 500℃ to obtain the precursor amorphous glass.
[0062] As can be seen from the X-ray diffraction peaks in Figure 1, there are no crystal diffraction peaks in the precursor amorphous glass prepared in Comparative Example 1, indicating that the prepared glass is amorphous glass.
[0063] The precursor amorphous glass prepared in Comparative Example 1 still has excellent transparency when the thickness is 3 mm (see Figure 2, where the word "Glass" can be seen).
[0064] Under 365 nm wavelength violet light excitation, the precursor amorphous glass prepared in Comparative Example 1 exhibited bright yellow luminescence. The normalized excitation and emission spectra at room temperature, measured using an Edinburgh FS980 fluorescence spectrometer, are shown in Figure 3. Eu can be observed in the emission spectrum. 2+ 4f of ions 6 5d 1 -4f 7 The transition is typically a broad-peak emission, but some also correspond to Eu. 3+ The emission peak is located at 588 nm. Its emission center wavelength is located at 588 nm, the excitation spectrum covers a wide band of 250-500 nm, and the excitation peak is located at 400 nm.
[0065] Comparative Example 2
[0066] A method for preparing glass includes the following steps:
[0067] S1. Weigh the required raw materials SiO2, SrO and Eu2O3 according to the molar fractions of 45mol% SiO2, 54.9mol% SrO and 0.1mol% Eu2O3, and mix and grind them for 30 minutes. Place the uniformly mixed and ground raw materials in a crucible.
[0068] S2. Place the crucible containing the raw material into a large covered crucible filled with activated carbon powder as a reducing atmosphere, keep it at 1400℃ in a muffle furnace for 1 hour, and then slowly cool it to room temperature in the muffle furnace for 8 hours to obtain the product.
[0069] Because the melting temperature was too low, this comparative example could not produce bulk microcrystalline glass.
[0070] Comparative Example 3
[0071] A method for preparing amorphous glass includes the following steps:
[0072] S1, the required raw materials SiO2, BaO, Eu2O3 were weighed according to the molar fractions of 70 mol% SiO2, 29.5 mol% SrO and 0.5 mol% Eu2O3, and mixed and ground for 30 min, and the mixed and ground uniform raw materials were placed in a crucible;
[0073] S2, the crucible containing the raw materials was placed in a large crucible covered with activated carbon powder as a reducing atmosphere, and was kept at 1600℃ for 1 h to melt, and after melting, the muffle furnace was slowly cooled from 1600℃ to room temperature over 8 hours, to obtain a blocky amorphous glass.
[0074] The XRD pattern of the amorphous glass prepared in the present comparative example is shown in Figure 14. As can be seen from the X-ray diffraction peaks in Figure 14, there is no crystal diffraction peak in the amorphous glass prepared in the present comparative example, indicating that the amorphous glass is prepared.
[0075] Example 1
[0076] A transparent microcrystalline glass comprising α-Sr2SiO4:Eu 2+ a single crystal phase.
[0077] A method for preparing a transparent microcrystalline glass, comprising the following steps:
[0078] S1, the required raw materials SiO2, BaO, Eu2O3 were weighed according to the molar fractions of 70 mol% SiO2, 29.5 mol% SrO and 0.5 mol% Eu2O3, and mixed and ground for 30 min, and the mixed and ground uniform raw materials were placed in a crucible;
[0079] S2, the crucible containing the raw materials was placed in a large crucible covered with activated carbon powder as a reducing atmosphere, and was kept at 1600℃ for 1 h to melt, and after melting, the muffle furnace was slowly cooled from 1600℃ to room temperature over 8 hours, to obtain a blocky amorphous glass. 2+ a single crystal phase.
[0080] As can be seen from the X-ray diffraction peaks in Figure 4, in the transparent microcrystalline glass prepared in the present example, α-Sr2SiO4:Eu 2+ a single crystal phase.
[0081] The transparent microcrystalline glass prepared in the present example still has a certain transparency when the thickness is 2 mm (see (a) in Figure 5), and further observation under a scanning electron microscope SEM shows that the microcrystalline glass containing 2-10 μm spot-shaped crystal morphology is successfully prepared (see Figure 6).
[0082] The transparent glass-ceramics prepared in this embodiment show bright green luminescence under 365 nm wavelength violet light excitation. The normalized excitation and emission spectra of the transparent glass-ceramics at room temperature were measured by Edinburgh FS980 fluorescence spectrometer and are shown in Figure 7. The emission spectrum shows a typical broad peak with a center wavelength of 532 nm, and the excitation spectrum covers a wide wavelength range of 250-450 nm with a peak at 365 nm. 2+ 4f 6 5d 1 -4f 7 transition, and a typical broad peak emission with a center wavelength of 532 nm, and the excitation spectrum covers a wide wavelength range of 250-450 nm with a peak at 365 nm.
[0083] Example 2
[0084] A transparent glass-ceramics, comprising α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phases.
[0085] A method for preparing a transparent glass-ceramics, comprising the following steps:
[0086] S1. The required raw materials SiO2, SrO and Eu2O3 are weighed according to the molar fractions of 45 mol% SiO2, 54.9 mol% SrO and 0.1 mol% Eu2O3, and mixed and ground for 30 min. The mixed and ground raw materials are placed in a crucible.
[0087] S2. The crucible containing the raw materials is placed in a large crucible covered with activated carbon powder as a reducing atmosphere, and is heated at 1600 ℃ in a muffle furnace for 1 h to melt. After melting, the muffle furnace is slowly cooled from 1600 ℃ to room temperature over 8 h to obtain a block-shaped transparent glass-ceramics containing α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phases.
[0088] As can be seen from the X-ray diffraction peaks in Figure 4, the transparent glass-ceramics prepared in this embodiment has precipitated α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phases.
[0089] The transparent glass-ceramics prepared in this embodiment still has certain transparency when the thickness is 2 mm (see (b) in Figure 5), and further observation under a scanning electron microscope SEM shows that the glass-ceramics containing 2-10 μm spot-shaped crystal morphology is successfully prepared (see Figure 8).
[0090] The transparent microcrystalline glass prepared in the embodiment exhibits bright green light under excitation of 365 nm wavelength violet light. The normalized excitation and emission spectra of the transparent microcrystalline glass at room temperature are shown in Figure 9 measured by Edinburgh FS980 fluorescence spectrometer. The emission spectrum can observe the typical broad peak emission of Eu 2+ 4f 6 5d 1 -4f 7 transition, and the center wavelength is located at 532 nm. The excitation spectrum covers a wide wavelength range of 250-450 nm, and the excitation peak is located at 365 nm.
[0091] Figure 10 is a variable temperature spectrum of the transparent microcrystalline glass of Example 2 at 300K-520K. It can be directly observed that the transparent microcrystalline glass still retains 70% of the initial luminescence intensity at 423.15K, further verifying that the transparent fluorescent microcrystalline glass has good thermal stability.
[0092] Example 3
[0093] A transparent microcrystalline glass, comprising α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phases.
[0094] A preparation method of a transparent microcrystalline glass, comprising the following steps:
[0095] S1, the required raw materials SiO2, SrO and Eu2O3 are weighed according to the molar fractions of 45mol% SiO2, 54.6mol% SrO and 0.4mol% Eu2O3, and mixed and ground for 30min. The mixed and ground uniform raw materials are placed in a crucible;
[0096] S2, the crucible containing the raw materials is placed in a large crucible covered with activated carbon powder as a reducing atmosphere, and is heated at 1600℃ in a muffle furnace for 1h to melt. After melting, the muffle furnace is slowly cooled from 1600℃ to room temperature for 8h, to obtain a block-shaped transparent microcrystalline glass containing α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phases.
[0097] As can be seen from the X-ray diffraction peaks in Figure 4, the transparent microcrystalline glass prepared in the embodiment has precipitated α-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ double crystal phases.
[0098] The transparent glass-ceramics prepared in this embodiment show bright green luminescence under 365 nm wavelength violet light excitation, and the normalized excitation and emission spectra thereof at room temperature measured by Edinburgh FS980 fluorescence spectrometer are shown in Figure 11; the emission spectrum can observe the typical broad peak emission of Eu 2+ ions, 4f 6 5d 1 -4f 7 transition, with the center wavelength at 532 nm, the excitation spectrum covering a wide band of 250-450 nm, and the excitation peak at 365 nm.
[0099] Embodiment 4
[0100] A transparent glass-ceramics, comprising β-Sr2SiO4:Eu 2+ single crystal phase.
[0101] A preparation method of the transparent glass-ceramics, comprising the following steps:
[0102] S1, weighing 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, and mixing and grinding for 30 min, and placing the mixed and ground raw materials in a crucible;
[0103] S2, placing the crucible containing the raw materials in a covered large crucible filled with activated carbon powder as a reducing atmosphere, and melting the raw materials at 1600 ℃ in a muffle furnace for 1 h, and slowly cooling the muffle furnace from 1600 ℃ to room temperature for 8 h after melting, to obtain a block-shaped transparent glass-ceramics containing β-Sr2SiO4:Eu 2+ single crystal phase.
[0104] As can be seen from the X-ray diffraction peaks in Figure 4, the transparent glass-ceramics prepared in this embodiment has precipitated β-Sr2SiO4:Eu 2+ single crystal phase.
[0105] The transparent glass-ceramics prepared in this embodiment still has certain transparency when the thickness is 2 mm (see (c) in Figure 5), and further observation under a scanning electron microscope SEM shows that the glass-ceramics containing 2-10 μm spot-shaped crystal morphology is successfully prepared (see Figure 12).
[0106] The transparent glass-ceramics prepared in this embodiment shows bright yellow-green luminescence under 365 nm wavelength violet light excitation, and the normalized excitation and emission spectra thereof at room temperature measured by Edinburgh FS980 fluorescence spectrometer are shown in Figure 13; the emission spectrum can observe the typical broad peak emission of Eu 2+ ions, 4f 6 5d 1 -4f 7The transition is a typical broad peak emission, with the center wavelength at 500 nm, the excitation spectrum covering a wide band of 250-450 nm, and the excitation peak at 325 nm.
[0107] A display device comprising the transparent glass-ceramic of embodiment 1.
[0108] A lighting device comprising the transparent glass-ceramic of embodiment 2.
[0109] On the basis of the above embodiments, and within the scope of protection claimed by the present application, the technical solutions of the present application can be changed, for example, the amount of raw materials, temperature and time, etc. without the need for creative labor improvements, which all belong to the protection scope of the present application.
Claims
1. A transparent microcrystalline glass, characterized in that, including a-Sr2Si04:Eu 2+ single-crystal phase transparent glass-ceramics, β-Sr2Si04:Eu 2+ single-crystal phase transparent glass-ceramics, or a-Sr2Si04:Eu 2+ and β-Sr2Si04:Eu 2+ at least one of the double-crystal phases.
2. The transparent microcrystalline glass according to claim 1, characterized in that, said a-Sr2Si04:Eu 2+ The single crystal phase has a spot-like crystal morphology; and / or, said a-Sr2Si04:Eu 2+ The single crystal phase has a spot-like crystal morphology; and / or, said a-Sr2Si04:Eu 2+ and β-Sr2Si04:Eu 2+ The double crystal phase has a spot-like crystal morphology.
3. The transparent microcrystalline glass according to claim 1, wherein said a-Sr2SiO4:Eu 2+ monocrystalline phase transparent glass-ceramics, β-Sr2SiO4:Eu 2+ monocrystalline phase transparent glass-ceramics, a-Sr2SiO4:Eu 2+ and β-Sr2SiO4:Eu 2+ The grain length of the bicrystalline phase is 1-12 μm.
4. The transparent microcrystalline glass according to claim 1, wherein The transparent microcrystalline glass can emit a broadband spectrum of light in the 400-700 nm band under excitation by 365 nm light.
5. The transparent microcrystalline glass according to claim 1, wherein The quantum efficiency of the transparent microcrystalline glass is not less than 74%.
6. The transparent microcrystalline glass according to claim 1, wherein The transparent microcrystalline glass still retains more than 70% of the initial light emission intensity at 150 DEG C.
7. The method of producing a transparent microcrystalline glass according to any one of claims 1 to 6, characterized in that, The method comprises the following steps: The SiO2, SrO and Eu2O3 raw materials are weighed and mixed, and then melted under a reducing atmosphere, and then cooled 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%, and the molar percentage of SrO is greater than the molar percentage of SiO2. The melting temperature is higher than 1510 DEG C.
8. The preparation method according to claim 7, characterized in that, In the raw materials, the molar percentage of Eu2O3 is 0.01-2%.
9. The preparation method according to claim 7, characterized in that, The melting temperature is 1570-1640 DEG C, and the temperature is maintained for 0.8-6 hours at the melting temperature of 1570-1640 DEG C; and / or the reducing atmosphere is selected from at least one of H2, CO or carbon powder.
10. A display or illumination device, characterized in that The transparent microcrystalline glass according to any one of claims 1-6.
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