CN112340982B - Composite glass material and preparation and application thereof - Google Patents
Composite glass material and preparation and application thereof Download PDFInfo
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- CN112340982B CN112340982B CN202011005789.1A CN202011005789A CN112340982B CN 112340982 B CN112340982 B CN 112340982B CN 202011005789 A CN202011005789 A CN 202011005789A CN 112340982 B CN112340982 B CN 112340982B
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
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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
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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Abstract
The invention discloses a composite glass material and preparation and application thereof. The composite glass material consists of a glass matrix and Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ Fluorescent powder composition; wherein, lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The mass ratio of the fluorescent powder is 7:1, and the glass matrix comprises the following components: 45-55wt% of SiO 2 ,25‑35wt%B 2 O 3 ,5‑15wt%CaO,10‑20wt%Na 2 O, the sum of the mass fractions of the components is 100wt%; the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The microstructure of the composite glass material is characterized by Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ Fluorescent powder is embedded in the glass substrate, and the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Lu in composite glass material 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The total mass percentage content of the fluorescent powder is 10-70wt%. The invention provides application of the composite glass material in preparing an LD device, and high laser saturation threshold and lumen flux are realized.
Description
Technical Field
The invention relates to a PiG Glass (Phosphor-in-Glass) and a preparation method thereof and application thereof in preparing LD devices, belonging to the field of solid luminescent materials.
Background
Driven by the tremendous demand and rapid growth of WLEDs, in recent years, various approaches have been exploredYellow or green emitting phosphors are incorporated into PiG (Phosphor-in-Glass) in a low melting Glass matrix. Primarily because of its unique advantages in luminescence and life cycle. Phosphor-embedded polymer converters are generally associated with severe aging and diminished luminescence over long periods of operation compared to conventional LEDs, and PiG exhibits excellent heat dissipation and resistance and simple operation in WLED fabrication. The preparation of PiG becomes easier and more economical without complicated production processes and hard synthesis such as under conditions of high temperature and high pressure, etc., which makes the PiG-based LED more competitive with LEDs produced by filling phosphor powder dispersed in silicone resin (PiS). However, piG also has congenital defects, lacking the red-emitting component, which is why LEDs are low in color. The luminescence resulting from low Color Rendering Index (CRI) and high Correlated Color Temperature (CCT) is strongly irritating to the human eye. Therefore, the research on warm white is imperative and significant. Currently, CN105399325A discloses Ce: YAG fluorescent glass for white light LED and a preparation method thereof, which is characterized in that PbO and B are mixed 2 O 3 ZnO and SiO 2 The raw materials are uniformly mixed, then high-temperature melting (about 1000 ℃) and water quenching are carried out to obtain glass slag, and the ground glass powder and YAG and Ce fluorescent powder are mixed and sintered into the fluorescent glass. The toxic raw material PbO is used in the production of the fluorescent glass, which is not beneficial to safe production. In addition, the white light packaged by the fluorescent glass is cold white light, has higher color temperature and lower display index, and cannot be applied to the field of indoor illumination. The patent CN107265873A discloses a low-melting-point fluorescent glass sheet for white light LED packaging and a preparation method thereof, and is characterized in that B 2 O 3 、ZnO、SiO 2 、Na 2 CO 3 、CaCO 3 And Al 2 O 3 The raw materials are uniformly mixed, then high-temperature melting (1100-1200 ℃) is carried out, the glass liquid is poured on a grinding tool to obtain matrix glass, and then the matrix glass is ground into micron-sized glass powder which is mixed with YAG: and uniformly mixing the Ce yellow fluorescent powder and sintering to obtain the fluorescent glass. The fluorescent glass has low transparency, more components, complicated and time-consuming preparation process and relatively high cost, and light obtained by doping single yellow fluorescent powder is cold white light which cannot be applied to the fields with high requirements on high color rendering index and low color rendering indexThe field of lighting of color temperature. Therefore, there is a great commercial interest in developing a fluorescent glass encapsulant for high-color-rendering index, low-color-temperature, warm-white LEDs.
It can be said that LED lighting is developing towards special lighting, and the requirements for high-power lighting devices in terms of high brightness, long life, and irradiation distance are increasingly high. Compared with LED illumination, laser illumination (LD) has higher efficiency and brightness and better modulability, can improve the brightness by increasing input power, and the high temperature and high heat generated by high power all put higher requirements on the heat conductivity, the reliability and the packaging mode of materials. Accordingly, methods of using a blue Laser Diode (LD) in combination with a color converter have been proposed in the fields of displays, projectors, headlights and other special illumination for achieving ultra-high brightness by consuming relatively low power.
The invention provides a method for preparing CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The fluorescent powder is prepared, and the luminescent performance of the material is regulated and controlled by selecting and designing glass components; the orange PiG is successfully prepared by adopting a melting heat treatment method, and under the excitation radiation of blue light, the white LD with high color rendering index (Ra is more than 90) can be realized, so that the orange PiG can be applied to the illumination field requiring high color rendering index and low color temperature, and a material of an LD device with high laser saturation threshold is expected to be developed, thereby realizing the controllable preparation of high-performance fluorescent glass and meeting the use of high-quality automobile lamp illumination devices.
Disclosure of Invention
The invention aims to provide CaAlSiN with high luminous intensity, high brightness, low melting temperature, stable product color, good color reducibility and excellent chemical stability 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ A composite glass material.
The second technical problem to be solved by the invention is to provide CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ A preparation method of a composite glass material.
The third purpose of the invention is to provide the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The application of the composite glass material in preparing LD devices is to realize high laser saturation threshold and lumen flux.
The invention adopts the technical scheme for solving the problems that:
in a first aspect, the invention provides a CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Composite glass material, said CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The composite glass material consists of glass base and Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ Fluorescent powder composition; wherein, lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The mass ratio of the fluorescent powder is 7:1, and the glass matrix comprises the following components: 45-55wt% of SiO 2 ,25-35wt%B 2 O 3 ,5-15wt%CaO,10-20wt%Na 2 O, the sum of the mass fractions of the components is 100wt%; the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The microstructure of the composite glass material is characterized by Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ Fluorescent powder is embedded in the glass substrate, and the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Lu in composite glass material 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The total mass percentage content of the fluorescent powder is 10-70wt%.
The CaAlSiN of the invention 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Composite glass material, due to the selection of SiO 2 -B 2 O 3 -CaO-Na 2 O glass matrix of Lu 3 Al 5 O 12 :Ce 3+ 、CaAlSiN 3 :Eu 2+ After the phosphor is dispersed in the glass matrix to form the PiG, the performance of the PiG is hardly affected by the phosphor. Preferably, the glass baseThe composition of the body is: 48wt% of SiO 2 ,27wt%B 2 O 3 ,10wt%CaO,15wt%Na 2 O。
The CaAlSiN of the invention 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Composite glass material using Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The fluorescent powder is mixed according to the mass ratio of 7:1, and white light can be directly realized when the burnt PiG and the blue light chip are compounded according to the mixture ratio. With Lu 3 Al 5 O 12 :Ce 3+ 、CaAlSiN 3 :Eu 2+ The increase of the content of the fluorescent powder increases the luminous intensity of the PiG. Most preferably, the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Lu in composite glass material 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The total mass percentage content of the fluorescent powder is 10wt%.
In a second aspect, the present invention provides a CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The preparation method of the composite glass material comprises the following steps:
(1) Mixing raw materials: mixing SiO 2 、B 2 O 3 、CaO、Na 2 Weighing O powder according to the component proportion, putting the O powder into a crucible, uniformly mixing, heating to 1300-1500 ℃, preserving heat for 10-30min, and carrying out melt quenching to obtain precursor glass;
(2) Preparation: grinding the precursor glass obtained in the step (1) into powder, and adding Lu in proportion 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The fluorescent powder is evenly ground and then put on the glass coated with the nano Al 2 O 3 Putting the crucible into a high-temperature melting furnace, heating to 600-900 ℃, preserving heat for 10-20min for melting and forming, and then cooling along with the furnace to obtain CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ A composite glass material.
In the present invention, use is made ofIs coated with nano Al 2 O 3 The crucible of the layer is obtained by easy demoulding of the prepared sample, and the nano Al 2 O 3 The layers act as spacers. Preferably, the crucible used is a corundum crucible.
Preferably, in step (1), the melting temperature is 1300 ℃ and the holding time is 15min.
Preferably, in the step (2), the melting temperature is 600-900 ℃, wherein the composite fluorescent glass fired at 850 ℃ is the best.
Preferably, in the step (2), the melting time is 10-20 minutes, wherein the composite fluorescent glass fired for 15min is optimal.
The shape of the composite fluorescent glass prepared by the invention can be plane, concave and convex, and the composite fluorescent glass can be cut, ground and polished without affecting the property of the composite fluorescent glass.
In a second aspect, the invention provides the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The composite glass material is applied to preparing an LD device excited by a blue-light LD chip.
The invention has the advantages that:
(1) Compared with the prior art, the invention uses B 2 O 3 -SiO 2 -Na 2 O-CaO is used as a matrix glass system, and Lu is added 3 Al 5 O 12 :Ce 3+ 、CaAlSiN 3 :Eu 2+ The fluorescent powder is prepared in the air by a low-temperature co-firing technology without atmosphere protection to obtain the composite fluorescent glass. The composite fluorescent glass prepared by the process has the advantages of high luminous intensity, high brightness, low melting temperature, stable product color, high color rendering index, good color reducibility and excellent chemical stability. In addition, the composite fluorescent glass prepared by the preparation method has simple process and low cost, and is suitable for industrial production.
(2) The white light LD device prepared by the composite fluorescent glass has high laser saturation threshold and lumen flux.
The invention is further described with reference to the drawings and the detailed description.
Drawings
FIG. 1: different Lu prepared for example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ An X-ray diffraction (XRD) pattern of the doped amount of the PiG sample; the right inset is a photograph under normal light and ultraviolet.
FIG. 2: different Lu prepared for example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ Fluorescence (PL) profile of doped quantity of PiG samples.
FIG. 3: 50wt% Lu prepared for example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ HRTEM of PiG.
FIG. 4: 50wt% Lu prepared for example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ PiG (LuAG: CASN-PiG) and Lu 3 Al 5 O 12 :Ce 3+ (LuAG) and CaAlSiN 3 :Eu 2+ Comparison of thermal stability of phosphor (CASN).
FIG. 5: 50wt% Lu prepared for example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ CL spectrum.
FIG. 6: different Lu prepared for example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ Graph of the light flux versus incident power for the doped quantity of the PiG sample.
Detailed Description
The present invention is described in detail below by way of examples, which are intended to be illustrative only and are not to be construed as limiting the scope of the invention, which is to be given the full breadth of the appended claims and any and all insubstantial modifications and variations thereof which can be made by a person skilled in the art in light of the above teachings.
Example 1
27g B is weighed 2 O 3 、48g SiO 2 、15g Na 2 Mixing O and 10g CaO, grinding uniformly, placing into a corundum crucible, placing into a high temperature furnace, heating to 1300 ℃, keeping the temperature for 15min, pouring into cold water, and quenching to obtain a precursorAnd (3) glass. Grinding the obtained precursor glass into powder, and respectively adding Lu 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ Grinding the phosphor (with the mass ratio of 7:1) to make the total mass of the phosphor account for 10wt%, 20wt%, 30wt%, 40wt%, 50wt%, 60wt% and 70wt% of the total mass of the phosphor and the precursor glass, and placing the ground phosphor on the glass coated with the nano Al 2 O 3 Putting the crucible into a high-temperature melting furnace, heating to 850 ℃, keeping the temperature for 15min, melting and forming, and cooling along with the furnace to obtain CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ A composite glass material.
FIG. 1 shows different Lu's prepared in example 1 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ X-ray diffraction (XRD) pattern of doped amount of PiG sample, detected in XRD spectrum with Lu 3 Al 5 O 12 :Ce 3+ The characteristic diffraction peak (PDF # 18-0761) of the cubic garnet structure is consistent, and the diffraction peak is gradually enhanced along with the increase of the content of the fluorescent powder. Due to CaAlSiN 3 :Eu 2+ The content is low, and only CaAlSiN can be detected on diffraction peaks 3 :Eu 2+ (002) The noodle is prepared from noodle (201).
As shown in FIG. 2, PL emission intensity gradually increased with the increase of the phosphor content in the glass matrix, but fluorescence quenching occurred when the phosphor content exceeded 50 wt%. And the sample showed typical Ce 3+ (5 d1-4 f) broad band emission with peak at 520nm, eu 2+ (5 d1-4 f) broadband emission, peak at 625nm.
As shown in fig. 3, a clear grain boundary without a transition layer was observed between the phosphor particles and the amorphous glass matrix at the nano-scale, and thus, it can be concluded that there was no interfacial reaction between the glass matrix and the phosphor.
From FIG. 4, it can be seen that 3 Al 5 O 12 :Ce 3+ And CaAlSiN 3 :Eu 2+ Phosphor powder phase, lu 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ The overall emission intensity of the PiG showed excellent thermal stability,at 300 ℃ 41% of the initial value was retained.
The CL image (fig. 5) clearly shows the luminescence information of the sample on the micrometer scale, i.e. luminescent particles, i.e. spherical particles (Lu) 3 Al 5 O 12 :Ce 3+ ) And rod-shaped particles CaAlSiN 3 :Eu 2+ Is embedded in a non-emissive matrix.
Comparative example 1
According to 30wt% B 2 O 3 -30wt%SiO 2 Weighing each substance according to the proportion of-40wt% ZnO, mixing and grinding uniformly, placing into a corundum crucible, placing into a high-temperature furnace, heating to 1350 ℃, preserving heat for 10min, pouring into cold water, and quenching to obtain the precursor glass. Grinding the obtained precursor glass into powder, and respectively adding Lu 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ The fluorescent powder (the mass ratio of 7:1) makes the mass of the fluorescent powder account for 10wt%, 20wt%, 30wt%, 40wt%, 50wt%, 60wt% and 70wt% of the total mass of the fluorescent powder and the precursor glass, and the fluorescent powder is ground and placed on the glass coated with the nano Al 2 O 3 And (3) putting the crucible in the layer into a high-temperature melting furnace, heating to 800 ℃ and preserving heat for 10min, and finding that all samples cannot be regularly molded after being cooled along with the furnace, have a plurality of pores and are loose and irregular.
Example 2
CaAlSiN prepared according to the method of example 1 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The composite glass material is cut into 0.8mm thin slices to be coupled with a blue light LD chip, the composite fluorescent glass is excited by the blue light LD with the wavelength of 450nm, the power density is adjusted, and different Lu are tested 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ Laser saturation threshold of phosphor content PiG.
The test results are shown in fig. 6. The results show that all Lu thicknesses of 0.8mm 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ Samples with different concentrations all showed significant brightness saturation. The excitation saturation threshold is more easily reached with increasing phosphor content. Taking a sample with 10% of fluorescent powder and 0.8mm of thickness as an example, the optical power density is2.69W mm -2 At that time, no light emission saturation occurred, and 70% of the 0.8mm sample was 1.7W mm -2 The saturation threshold has been reached. 10wt% of PiG at 2.69W/mm 2 Can reach the luminous flux of 183.68lm under the incident power of the laser. The experimental result shows that the suitable Lu of the invention 3 Al 5 O 12 :Ce 3+ /CaAlSiN 3 :Eu 2+ The concentration of composite fluorescent glass (PiG) can reach a higher saturation threshold, and the PiG has potential application in blue light LD converters.
The present invention is not limited to the above-described embodiments, and various changes or modifications of the present invention are intended to be included within the scope of the present invention if they fall within the claims and equivalent technical scope of the present invention.
Claims (5)
1. CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The application of the composite glass material in preparing an LD device excited by a blue-light LD chip is characterized in that: the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The composite glass material consists of glass matrix and Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ Fluorescent powder; wherein, lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The mass ratio of the fluorescent powder is 7:1, and the glass matrix comprises the following components: 48wt% SiO 2 ,27 wt% B 2 O 3 ,10 wt% CaO,15 wt%Na 2 O; the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The microstructure of the composite glass material is characterized by Lu 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ Fluorescent powder is embedded in the glass substrate, and the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ Lu in composite glass material 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The total mass percentage content of the fluorescent powder is 10wt%.
2. The use of claim 1, wherein: the CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ The preparation method of the composite glass material comprises the following steps:
(1) Mixing raw materials: mixing SiO 2 、B 2 O 3 、CaO、Na 2 Weighing O powder according to the component proportion, putting the O powder into a crucible, uniformly mixing, heating to 1300-1500 ℃, preserving heat for 10-30min, and carrying out melt quenching to obtain precursor glass;
(2) Preparation: grinding the precursor glass obtained in the step (1) into powder, and adding Lu in proportion 3 Al 5 O 12 :Ce 3+ Phosphor and CaAlSiN 3 :Eu 2+ The fluorescent powder is evenly ground and then is coated with the nano Al 2 O 3 Putting the crucible into a high-temperature melting furnace, heating to 600-900 ℃, preserving heat for 10-20min for melting and forming, and then cooling along with the furnace to obtain CaAlSiN 3 :Eu 2+ /Lu 3 Al 5 O 12 :Ce 3+ A composite glass material.
3. The use of claim 2, wherein: the crucible used was a corundum crucible.
4. Use according to claim 2, characterized in that: in the step (1), the melting temperature is 1300 ℃, and the heat preservation time is 15min.
5. Use according to claim 2, characterized in that: in the step (2), the melting temperature is 850 ℃, and the heat preservation time is 15min.
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