A fluorescent microcrystal, a glass-ceramic film composite material and a preparation method and application thereof
By preparing a glass-ceramic film composite material of Lu1.9Mg2Al2-xGaxSi2O12:0.1Ce3+ micron-sized crystals, the problem of light saturation of fluorescent microcrystals under blue laser excitation was solved, achieving warm white light emission and high-efficiency luminescence, which is suitable for warm white laser illumination.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- MINDU INNOVATION LAB
- Filing Date
- 2022-10-27
- Publication Date
- 2026-07-14
AI Technical Summary
Existing fluorescent microcrystals are prone to light saturation under blue laser excitation, causing the luminescence intensity to no longer increase or decrease, making it impossible to effectively achieve warm white light emission, which affects the lighting effect and human eye health.
A glass-ceramic film composite material of Lu1.9Mg2Al2-xGaxSi2O12:0.1Ce3+ micron-sized crystals was prepared. By selecting a matrix with a highly symmetric garnet structure and a Ce3+ nanosecond-level fluorescence lifetime, the emission wavelength was tuned to the orange-red light band, thereby improving the luminescence saturation threshold.
It effectively generates warm white light under blue laser excitation, improves luminous efficiency and color rendering index, reduces light saturation, and is suitable for warm white laser lighting.
Smart Images

Figure CN117945416B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of solid-state luminescent materials, and in particular to a fluorescent microcrystal, a glass-ceramic film composite material, its preparation method, and its application. Background Technology
[0002] In recent years, the demand for ultra-high luminous flux, high power, and miniaturized special lighting, such as high-end automotive headlights, aerospace lights, and deep-sea exploration lights, has increased rapidly, placing higher demands on white solid-state lighting technology. Emerging solutions based on blue laser-driven phosphor conversion materials to achieve ultra-high brightness white light (i.e., phosphor-converted white laser diode technology, pc-wLD) offer significantly improved illumination range and distance compared to white LED products. As the core component of pc-wLD, accelerating its research and development is crucial.
[0003] As is well known, the spectral distribution of white light illumination affects the luminescence quality. Because the spectrum of "blue laser + yellow fluorescent material" lacks red light components, it appears as cool white light, and long-term exposure can affect human eye health. The accuracy and speed of human vision improve with increasing color temperature and color rendering index; warm white light illumination offers better visibility and penetration, making the further development of a spectrally balanced warm white pc-wLD imperative. However, to date, fluorescent microcrystals with red light emission characteristics are mostly based on Eu... 2+ or Mn 4+ As a doping center, such as Mg2Al4Si5O 18 Eu 2+ CaAlSiN3:Eu 2+ K2SiF6:Mn 4+ Under blue laser excitation, fluorescent materials exhibit a significant luminescence saturation problem—that is, the luminescence intensity no longer increases with increasing incident laser intensity, and may even decrease. The reason for this is that their fluorescence lifetimes are on the order of microseconds or milliseconds. After electrons are pumped to the excited state level under high photon density laser irradiation, they are highly susceptible to ground-state bleaching, energy upconversion dominated by second-order nonlinear processes, and optically stimulated luminescence, thus inducing luminescence saturation. Summary of the Invention
[0004] To address the aforementioned problems, this invention prepares a Lu-containing material with stable structure and suitable optical properties. 1.9 Mg2Al 2- x Ga x Si2O 12 0.1Ce 3+ A glass-ceramic film composite material with x = 0.0-1.0 micrometer crystals. Its activation center Ce 3+Nanosecond-level fluorescence lifetime can effectively improve the luminescence saturation threshold; simultaneously, the matrix is selected from garnet-structured crystal phases (doped with Ce) which have high symmetry and a strong crystal field environment. 3+ Its lifetime is only tens of nanoseconds, which reduces Ce 3+ The 5d lowest orbital energy level can effectively control the emission wavelength to the orange-red light band, enabling it to emit warm white light under blue laser excitation, making it suitable for warm white laser illumination.
[0005] This invention proposes a Lu-containing 1.9 Mg2Al 2-x Ga x Si2O 12 0.1Ce 3+ The aim of this study is to prepare a glass-ceramic film composite material with x = 0.0-1.0 micrometer crystals, which has a stable structure, suitable optical properties, and can be used for warm white laser illumination as a fluorescent conversion material.
[0006] According to one aspect of this application, a fluorescent microcrystal is provided, the fluorescent microcrystal having the chemical formula Lu. 1.9 Mg2Al2Si2O 12 0.1Ce 3+ .
[0007] Optionally, the fluorescent microcrystal has the chemical formula Lu. 1.9 Mg2Al 2-x Ga x Si2O 12 0.1Ce 3+ , where x = 0.0 < x ≤ 1.0.
[0008] According to another aspect of this application, a method for preparing the above-mentioned fluorescent microcrystals is provided, comprising the following steps:
[0009] Raw materials containing Lu2O3, MgCO3, SiO2, CeO2, and Al2O3 are mixed and calcined to obtain the fluorescent microcrystals described in claim 1.
[0010] or;
[0011] Raw materials containing Lu2O3, MgCO3, SiO2, CeO2, Al2O3, and Ga2O3 are mixed and calcined to obtain the fluorescent microcrystals described in claim 2.
[0012] Preparation of Lu 1.9 Mg2Al2Si2O 12 0.1Ce 3+ When fluorescent micron crystals are formed,
[0013] The molar percentage of Lu2O3 in the raw materials is 15.70 mol%.
[0014] The molar percentage of MgCO3 was 33.06 mol%.
[0015] The molar percentage of SiO2 was 33.06 mol%.
[0016] The molar percentage of CeO2 was 1.65 mol%.
[0017] The molar percentage of Al2O3 was 16.53 mol%.
[0018] Optionally,
[0019] Preparation of Lu 1.9 Mg2Al 2-x Ga x Si2O 12 0.1Ce 3+ When micron-sized crystals are formed,
[0020] The molar percentage of Lu2O3 in the raw materials is 15.70 mol%.
[0021] The molar percentage of MgCO3 was 33.06 mol%.
[0022] The molar percentage of SiO2 was 33.06 mol%.
[0023] The molar percentage of CeO2 was 1.65 mol%.
[0024] The molar percentage of Al2O3 was 16.53 μmol%.
[0025] The molar percentage of Ga2O3 is y mol%; where 0.0 < y ≤ 8.265.
[0026] The roasting temperature is 1400–1500℃;
[0027] Optionally, the roasting temperature is any value or a range between 1400℃, 1410℃, 1420℃, 1430℃, 1440℃, 1450℃, 1460℃, 1470℃, 1480℃, 1490℃, and 1500℃.
[0028] The roasting time is 3 to 12 hours.
[0029] Optionally, the roasting time is any value among 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h, and 12h, or a range between any two.
[0030] Specifically, the present invention employs the following preparation process:
[0031] According to Lu 1.9 Mg2Al 2-x Ga x Si2O 12 0.1Ce 3+ The chemical formulas of the crystals with x = 0.0-1.0 micrometers were used to weigh the raw materials, and the corresponding molar percentages are as follows:
[0032] 15.70 mol% Lu₂O₃; 33.06 mol% MgCO₃; 33.06 mol% SiO₂; 1.65 mol% CeO₂; 16.53-y mol% Al₂O₃; y mol% Ga₂O₃, where y is 0.00-8.265 mol%. The powder raw materials were ground evenly according to the component ratio and placed in a crucible. The crucible was then placed in a tube furnace filled with a nitrogen-hydrogen mixture and held at 1400-1500℃ for 3-12 hours. After cooling in the furnace, the material was removed, pulverized, ground, and sieved to obtain Lu. 1.9 Mg2Al 2-x Ga x Si2O 12 0.1Ce 3+ , x = 0.0-1.0 fluorescent micron crystals.
[0033] According to another aspect of this application, a glass-ceramic film composite material is provided, comprising a substrate and a coating applied to the surface of the substrate;
[0034] The coating comprises organic slurry, fluorescent microcrystalline powder, and low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O.
[0035] The microcrystalline powder is selected from the fluorescent microcrystalline powder described above or the fluorescent microcrystalline powder prepared by the above preparation method.
[0036] The organic slurry contains terpineol, ethyl acetate, and ethyl cellulose;
[0037] The content of terpineol is 50 wt%.
[0038] The content of ethyl acetate is 46 wt%.
[0039] The content of ethyl cellulose is 4 wt%;
[0040] Optionally, the substrate is selected from aluminum nitride substrates with high thermal conductivity or transparent sapphire substrates.
[0041] According to another aspect of this application, a method for preparing the above-mentioned glass-ceramic film composite material is provided, comprising the following steps:
[0042] A coating containing the organic slurry, the fluorescent microcrystalline powder, and low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O is applied to the surface of the substrate, dried, and sintered to obtain the glass-ceramic film composite material.
[0043] The drying temperature is 300–350°C;
[0044] Optionally, the drying temperature is any value or a range between 300°C, 310°C, 320°C, 330°C, 340°C, and 350°C.
[0045] The drying time is 1 to 24 hours;
[0046] Optionally, the drying time is any value among 1h, 6h, 12h, 18h, and 24h, or a range between any two.
[0047] The sintering temperature is 690–750°C;
[0048] Optionally, the sintering temperature is any value or a range between 690°C, 700°C, 710°C, 720°C, 730°C, 740°C, and 750°C.
[0049] The sintering time is 0.25 to 1 hour.
[0050] Optionally, the sintering time is any value among 0.25h, 0.5h, 0.75h, and 1h, or a range between any two.
[0051] According to another aspect of this application, an application is provided of the above-described glass-ceramic membrane composite material or the glass-ceramic membrane composite material prepared by the above-described preparation method, characterized in that,
[0052] Fluorescent conversion material that generates warm white light under 455 nm high-power blue laser excitation for use in warm white laser illumination.
[0053] The advantages of this application are: measurements using a self-built laser illumination testing system show that the composite material can effectively generate warm white light under 455 nm high-power blue laser excitation. The material in this invention has advantages such as simple preparation, low cost, and suitable performance. Attached Figure Description
[0054] Figure 1 The Lu-containing sample obtained in Example 1 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+X-ray diffraction pattern of micron-crystalline glass-ceramic film composite material.
[0055] Figure 2 The Lu-containing sample obtained in Example 1 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Front scanning electron microscope image of micron-sized glass-ceramic film composite material.
[0056] Figure 3 The Lu-containing sample obtained in Example 1 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Cross-sectional scanning electron microscope image of microcrystalline glass-ceramic film composite material.
[0057] Figure 4 Under blue laser excitation as obtained in Example 1, Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Steady-state fluorescence decay spectrum of micron-crystalline glass-ceramic film composite material.
[0058] Figure 5 Under blue laser excitation as obtained in Example 1, Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Electroluminescence spectrum of micron-crystalline glass-ceramic film composite material.
[0059] Figure 6 Under blue laser excitation as obtained in Example 1, Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Luminescent photograph of a physical sample of a microcrystalline glass-ceramic film composite material.
[0060] Figure 7 Under blue laser excitation as obtained in Example 2, Lu-containing 1.9 Mg2Al2Si2O 12 0.1Ce 3+ Electroluminescence spectrum of micron-crystalline glass-ceramic film composite material.
[0061] Figure 8 Under blue laser excitation as obtained in Example 3, Lu-containing1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+ Electroluminescence spectrum of micron-crystalline glass-ceramic film composite material. Detailed Implementation
[0062] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments.
[0063] Unless otherwise specified, all raw materials used in the embodiments of this application were purchased through commercial channels.
[0064] Example 1
[0065] In this embodiment, the fluorescent microcrystalline phase contained in the composite material is Lu. 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Analytical-grade Lu₂O₃, MgCO₃, Al₂O₃, Ga₂O₃, SiO₂, and CeO₂ powders were mixed evenly in an agate mortar at a molar ratio of 15.70Lu₂O₃-33.06MgCO₃-12.40Al₂O₃-4.13Ga₂O₃-33.06SiO₂-1.65CeO₂. The mixture was then placed in an alumina crucible and placed in a tube furnace filled with a nitrogen-hydrogen mixture. The furnace was held at 1450℃ for 6 hours, followed by furnace cooling. The mixture was then removed, pulverized, ground, and sieved to obtain Lu₂O₃ powder. 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Micron-sized crystalline powder. Simultaneously, terpineol:ethyl acetate:ethyl cellulose were weighed in a ratio of 50wt%:46wt%:4wt%, and mixed at room temperature and 600 rpm to prepare an organic slurry. The organic slurry, low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O, and Lu were weighed according to a 1:1:1 mass ratio. 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Micron-sized crystalline powders were mixed and ground evenly in an agate mortar to obtain a coating slurry. This slurry was then coated onto a transparent sapphire substrate using an automated coating machine, and transferred to a 300°C oven for 1 hour to allow the organic matter to fully volatilize. Finally, it was sintered in a 690°C muffle furnace for 30 minutes to obtain a Lu-containing substrate. 1.9 Mg2Al1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Micron-sized glass-ceramic membrane composite materials.
[0066] Figure 1 The Lu-containing sample obtained in Example 1 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ X-ray diffraction pattern of micron-crystalline glass-ceramic film composite material.
[0067] Figure 2 The Lu-containing sample obtained in Example 1 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Front scanning electron microscope image of micron-sized glass-ceramic film composite material.
[0068] Figure 3 The Lu-containing sample obtained in Example 1 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Cross-sectional scanning electron microscope image of microcrystalline glass-ceramic film composite material.
[0069] Figure 4 Under blue laser excitation as obtained in Example 1, Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Steady-state fluorescence decay spectrum of micron-crystalline glass-ceramic film composite material.
[0070] Figure 5 Under blue laser excitation as obtained in Example 1, Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Electroluminescence spectrum of micron-crystalline glass-ceramic film composite material.
[0071] Figure 6 Under blue laser excitation as obtained in Example 1, Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+Luminescent photograph of a physical sample of a microcrystalline glass-ceramic film composite material.
[0072] X-ray diffraction data indicate that Lu-containing 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ In the micron-crystalline glass-ceramic film composite material, apart from the amorphous peaks exhibited by the glass matrix, the positions of the crystalline phase diffraction peaks are all consistent with the garnet structure Lu3Al5O 12 :Ce 3+ (ICSD NO.23846) Corresponding standard card, no stray signals (e.g.) Figure 1 (As shown). A front-side scanning electron microscope image of the composite material reveals Lu particles with a diameter of approximately 20 micrometers. 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ Microcrystals were embedded in a low-melting-point glass matrix. Auger electron spectroscopy (EDS) analysis revealed the presence of Lu, Mg, Al, Ga, Si, Ce, O and Si, B, Zn, Na, Al, O at the embedded particles and in the glass matrix, respectively, consistent with the elemental compositions of the microcrystals and the low-melting-point glass (e.g., ...). Figure 2 (As shown). Meanwhile, as... Figure 3 As shown, the glass-ceramic film exhibits excellent film-forming properties, and the glass-ceramic film and sapphire substrate are firmly bonded, with a film thickness of approximately 135 micrometers. Steady-state fluorescence decay spectroscopy indicates that this composite material has a fluorescence lifetime in the nanosecond range, at 67.25 nanoseconds (e.g., ...). Figure 4 As shown in the figure, because the time for electrons to return from the excited state to the ground state is extremely short, optical saturation is not easily achieved. Subsequently, using a self-built laser display testing system, the fluorescence intensity of Lu-containing lasers under blue laser excitation was measured. 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+ The electroluminescence spectrum of a micron-crystalline glass-ceramic film composite material, which can effectively produce warm white light under blue laser excitation, has a luminous flux of 295.7 lumens, a luminous efficacy of 65.7 lumens / watt, a color rendering index of 67.7, a color temperature of 3573K, and color coordinates of (0.4022, 0.3912). Figure 5 As shown). Figure 6 As shown, this demonstrates the effect of blue laser excitation on Lu-containing... 1.9 Mg2Al 1.5 Ga 0.5 Si2O 12 0.1Ce 3+A photograph of a physical sample of the micron-crystalline glass-ceramic film composite material shows bright, warm white light. All of the above data indicate that the material in this invention is a novel material that can be used for warm white laser illumination.
[0073] Example 2
[0074] In this embodiment, the fluorescent microcrystalline phase contained in the composite material is Lu. 1.9 Mg2Al2Si2O 12 0.1Ce 3+ Analytical-grade Lu₂O₃, MgCO₃, Al₂O₃, SiO₂, and CeO₂ powders were mixed evenly in an agate mortar at a molar ratio of 15.70 Lu₂O₃ - 33.06 MgCO₃ - 16.53 Al₂O₃ - 33.06 SiO₂ - 1.65 CeO₂. The mixture was then placed in an alumina crucible and placed in a tube furnace filled with a nitrogen-hydrogen mixture. The furnace was held at 1450°C for 6 hours, followed by furnace cooling. The mixture was then removed, pulverized, ground, and sieved to obtain Lu₂O₃ powder. 1.9 Mg2Al2Si2O 12 0.1Ce 3+ Micron-sized crystalline powder. Simultaneously, terpineol:ethyl acetate:ethyl cellulose were weighed in a ratio of 50wt%:46wt%:4wt%, and mixed at room temperature and 600 rpm to prepare an organic slurry. The organic slurry, low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O, and Lu were weighed according to a 1:1:1 mass ratio. 1.9 Mg2Al2Si2O 12 0.1Ce 3+ Micron-sized crystalline powders were mixed and ground evenly in an agate mortar to obtain a coating slurry. This slurry was then coated onto a transparent sapphire substrate using an automated coating machine, and transferred to a 300°C oven for 1 hour to allow the organic matter to fully volatilize. Finally, it was sintered in a 690°C muffle furnace for 30 minutes to obtain a Lu-containing substrate. 1.9 Mg2Al2Si2O 12 0.1Ce 3+ Micron-sized glass-ceramic membrane composite materials.
[0075] Figure 7 Under blue laser excitation as obtained in Example 2, Lu-containing 1.9 Mg2Al2Si2O 12 0.1Ce 3+ Electroluminescence spectrum of micron-crystalline glass-ceramic film composite material.
[0076] Using a self-built laser display testing system, the concentration of Lu under blue laser excitation was measured. 1.9 Mg2Al2Si2O12 0.1Ce 3+ The electroluminescence spectrum of a micron-crystalline glass-ceramic film composite material, which can effectively produce warm white light under blue laser excitation, has a luminous flux of 393.8 lumens, a luminous efficacy of 78.8 lumens / watt, a color rendering index of 68.6, a color temperature of 3897K, and color coordinates of (0.3896, 0.3949). Figure 7 As shown in the figure, it can be used for warm white laser illumination.
[0077] Example 3
[0078] In this embodiment, the fluorescent microcrystalline phase contained in the composite material is Lu. 1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+ Analytical-grade Lu₂O₃, MgCO₃, Al₂O₃, Ga₂O₃, SiO₂, and CeO₂ powders were mixed evenly in an agate mortar at a molar ratio of 15.70Lu₂O₃-33.06MgCO₃-8.265Al₂O₃-8.265Ga₂O₃-33.06SiO₂-1.65CeO₂. The mixture was then placed in an alumina crucible and placed in a tube furnace filled with a nitrogen-hydrogen mixture. The mixture was held at 1450℃ for 6 hours, then cooled in the furnace, removed, pulverized, ground, and sieved to obtain Lu₂O₃ powder. 1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+ Micron-sized crystalline powder. Simultaneously, terpineol:ethyl acetate:ethyl cellulose in a ratio of 50 wt%:46 wt%:4 wt% were weighed and mixed at room temperature and 600 rpm to prepare an organic slurry. The organic slurry, low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O, and Lu were weighed according to a 1:1:1 mass ratio. 1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+ Micron-sized crystalline powders were mixed and ground evenly in an agate mortar to obtain a coating slurry. This slurry was then coated onto a transparent sapphire substrate using an automated coating machine, and transferred to a 300°C oven for 1 hour to allow the organic matter to fully volatilize. Finally, it was sintered in a 690°C muffle furnace for 30 minutes to obtain a Lu-containing substrate. 1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+Micron-sized glass-ceramic membrane composite materials.
[0079] Figure 8 Under blue laser excitation as obtained in Example 3, Lu-containing 1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+ Electroluminescence spectrum of micron-crystalline glass-ceramic film composite material.
[0080] Using a self-built laser display testing system, the concentration of Lu under blue laser excitation was measured. 1.9 Mg2Al 1.0 Ga 1.0 Si2O 12 0.1Ce 3+ The electroluminescence spectrum of the micron-crystalline glass-ceramic film composite material shows that this material can effectively produce warm white light under blue laser excitation, with a luminous flux of 223.1 lumens, a luminous efficacy of 55.8 lumens / watt, a color rendering index of 66.9, a color temperature of 3161 K, and color coordinates of (0.4164, 0.3787). Figure 8 As shown in the figure, it can be used for warm white laser illumination.
[0081] The above description is merely a few embodiments of this application and is not intended to limit this application in any way. Although this application discloses preferred embodiments as described above, it is not intended to limit this application. Any changes or modifications made by those skilled in the art without departing from the scope of the technical solution of this application using the disclosed technical content are equivalent to equivalent implementation cases and fall within the scope of the technical solution.
Claims
1. A fluorescent microcrystal, characterized in that, The chemical formula of the fluorescent microcrystal is Lu. 1.9 Mg2Al 2-x Ga x Si2O 12 0.1Ce 3+ , where 0.0 < x ≤ 1.
0.
2. A method for preparing fluorescent microcrystals according to claim 1, characterized in that, Includes the following steps: Raw materials containing Lu2O3, MgCO3, SiO2, CeO2, Al2O3, and Ga2O3 are mixed and calcined to obtain the fluorescent microcrystals described in claim 1.
3. The preparation method according to claim 2, characterized in that, The molar percentage of Lu2O3 in the raw material is 15.70 mol%. The molar percentage of MgCO3 is 33.06 mol%; The molar percentage of SiO2 is 33.06 mol% The molar percentage of CeO2 is 1.65 mol%. The molar percentage of Al2O3 is 16.53 μmol%. The molar percentage of Ga2O3 is y mol%; where 0.0 < y ≤ 8.
265.
4. The preparation method according to claim 2, characterized in that, The roasting temperature is 1400~1500℃; The roasting time is 3 to 12 hours.
5. A glass-ceramic membrane composite material, characterized in that, Includes the substrate and the coating applied to the surface of the substrate; The coating comprises organic slurry, fluorescent microcrystalline powder, and low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O. The fluorescent microcrystal powder is selected from the fluorescent microcrystals described in claim 1 or the fluorescent microcrystals prepared by the preparation method described in any one of claims 2 to 4.
6. The glass-ceramic membrane composite material according to claim 5, characterized in that, The organic slurry contains terpineol, ethyl acetate, and ethyl cellulose; The content of terpineol is 50 wt%. The content of ethyl acetate is 46 wt%; The content of ethyl cellulose is 4 wt%.
7. The glass-ceramic membrane composite material according to claim 5, characterized in that, The substrate is selected from aluminum nitride substrate or transparent sapphire substrate.
8. A method for preparing the glass-ceramic membrane composite material according to any one of claims 5-7, Its features are, Includes the following steps: A coating containing the organic slurry, the fluorescent microcrystals, and low-melting-point glass powder with a molar percentage of 38SiO2-40B2O3-4ZnO-4Na2O-3Al2O3-1Li2O is applied to the surface of the substrate, dried, and sintered to obtain the glass-ceramic film composite material.
9. The preparation method according to claim 8, characterized in that, The drying temperature is 300~350℃; The drying time is 1~24 hours; The sintering temperature is 690~750℃; The sintering time is 0.25~1h.
10. The application of a glass-ceramic membrane composite material according to any one of claims 5-7 or a glass-ceramic membrane composite material prepared by the preparation method according to any one of claims 8 or 9, characterized in that, Fluorescent conversion material that generates warm white light under 455 nm high-power blue laser excitation for use in warm white laser illumination.