CN112851124B - Glass ceramic membrane composite material for laser illumination - Google Patents

Glass ceramic membrane composite material for laser illumination Download PDF

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CN112851124B
CN112851124B CN202110154403.1A CN202110154403A CN112851124B CN 112851124 B CN112851124 B CN 112851124B CN 202110154403 A CN202110154403 A CN 202110154403A CN 112851124 B CN112851124 B CN 112851124B
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glass ceramic
composite material
ceramic membrane
mixture
membrane composite
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CN112851124A (en
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林世盛
林航
徐桔
王元生
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • C04B41/5023—Glass-ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
    • C04B41/61—Coating or impregnation
    • C04B41/65—Coating or impregnation with inorganic materials

Abstract

The invention provides a fertilizer containing (Lu)2M)(Al4Si)O12:Ce3+A micron crystal glass ceramic membrane composite material aims to prepare a fluorescent conversion material which has a stable structure and can be used for laser illumination, and relates to the field of luminescent materials. The material disclosed by the invention has appropriate optical properties, and has the advantages of simple preparation process, batch preparation, adjustable spectrum width and the like. The composite material can effectively generate white light under the excitation of 455-nanometer high-power blue laser due to the rapid conduction effect of the high-thermal-conductivity transparent sapphire substrate in the composite material on a large amount of heat at a light spot.

Description

Glass ceramic membrane composite material for laser illumination
Technical Field
The invention relates to the field of solid luminescent materials, in particular to a glass ceramic membrane composite material capable of being applied to laser illumination.
Background
In recent years, with the continuous promotion of domestic infrastructure construction and the gradual improvement of the living standard of people, the requirements of high-power special illumination and high-power display of high-end headlamps in front of a vehicle, high-end projectors, mining lamps, high-pole lamps in squares/ports and the like with light flux up to thousands of lumens or even tens of thousands of lumens are rapidly increased, and the demand of ultrahigh-power white light solid state illumination and display is increasingly huge. However, the current single-chip white LED has a phenomenon of "efficiency dip" caused by electron-hole auger recombination, so that its power is low and brightness is low, and it is obviously unable to directly meet the application requirements. In contrast, researchers usually package multiple chips into one module to improve the power and the luminance of the white LED, but this may cause the problems of reduced device stability, reduced lighting efficiency of the lamp, complicated lamp design, and the like, and significantly increases the cost. In order to obtain a high-quality high-power solid-state light source, attention is paid to a blue Laser Diode (LD). Compared with the conventional LED technology, the blue LD has many advantages if it is used as an excitation source of the phosphor powder meeting the requirements. Under the condition of high input power density, the electro-optic conversion efficiency of the LD is high, and the problem of efficiency dip is avoided; moreover, the light yield on the unit chip area is higher, the light emitting directivity is good, the energy density is high, and the LED light source is particularly suitable for an ultrahigh-brightness white light source with small optical expansion; the monochromaticity is better, and the proper fluorescent powder is easy to match; the structure is more compact, and the design of the terminal illuminating body has more freedom. However, since the laser light emitting diode has an ultra-high power density, a large amount of heat is generated at a light spot during the working process, the requirement on the used fluorescent conversion material is extremely high, and the available material is very deficient. In this context, there is a need to develop a fluorescence conversion material that can be applied to laser illumination.
The present invention has been made to solve the above problems and to provide a stable structure of a complex of (Lu) and (Lu) having suitable optical properties2M)(Al4Si)O12:Ce3+A microcrystalline glass ceramic film composite material suitable for laser illumination.
Disclosure of Invention
The invention provides a fertilizer containing (Lu)2M)(Al4Si)O12:Ce3+A micron crystal glass ceramic membrane composite material aims to prepare a fluorescent conversion material which has a stable structure and can be applied to laser illumination.
The invention adopts the following preparation process:
(1) designing a precursor glass matrix, wherein the glass matrix comprises the following components in percentage by weight: 30-42 mol% SiO2；26-37mol％B2O3；5-15mol％Al2O3；5-15mol％Lu2O3；0.1-5mol％CeO2；xmol％MgCO3；ymol％CaCO3；zmol％SrCO3；wmol％BaCO3The total mole amount of the above components is 100 mol%, wherein MgCO is3、CaCO3、SrCO3、BaCO3X, y, z, w of (A) are defined by the corresponding target solid solution crystalline phase, i.e. (Lu)2M)(Al4Si)O12:Ce3+Wherein the solid solution ratio of one or more elements selected from Mg, Ca, Sr and Ba is determined, and the total mole amount of x + y + z + w is 5-25 mol%.
(2) Grinding the powder raw materials uniformly according to the component proportion, placing the powder raw materials into a crucible, placing the crucible into a 1450-1600 ℃ high-temperature furnace for heat preservation for 2 hours, then quickly pouring the glass melt into a copper mold, continuously carrying out heat treatment for 120 minutes at 520 ℃, crushing, grinding and sieving to obtain the product containing (Lu)2M)(Al4Si)O12:Ce3+Microcrystalline glass ceramic powder. Meanwhile, according to the weight ratio of terpineol: the ethyl cellulose is 97 wt% to 3 wt% and mixed and stirred at 80 deg.C and 600 rAn organic slurry mixture was obtained.
(3) Weighing the organic slurry mixture and the low-melting-point glass powder (10 SiO) according to the mass ratio of 1:1:12-35P2O5-24Al2O3-5Na2CO3-26K2CO3Mol%) and (Lu) and2M)(Al4Si)O12:Ce3+and (3) respectively and uniformly mixing and grinding the microcrystalline glass ceramic powder in an agate mortar to obtain coating slurry. Then, coating the slurry on a transparent sapphire substrate by a screen printing method, controlling the thickness by the screen printing times, transferring the coated substrate into a 300 ℃ oven, standing for 10 hours for glue removal to fully volatilize the organic mixture in the oven, and finally sintering in a 550 ℃ 700 ℃ muffle furnace for 20 minutes to obtain the product (Lu)2M)(Al4Si)O12:Ce3+Micron crystal glass ceramic membrane composite material.
The invention also relates to a fertilizer containing (Lu)2M)(Al4Si)O12:Ce3+The application of the micron crystal glass ceramic membrane composite material is characterized in that the micron crystal glass ceramic membrane composite material is used for laser illumination. The self-built laser lighting test system shows that the composite material can effectively generate white light under the excitation of 455-nanometer high-power blue laser due to the rapid conduction effect of the high-thermal-conductivity transparent sapphire substrate in the composite material on a large amount of heat at a light spot. The material disclosed by the invention has appropriate luminescence property, and has the advantages of simple preparation process, batch preparation, adjustable spectrum width and the like.
Drawings
FIG. 1: containing Lu2BaAl4SiO12:Ce3+X-ray diffraction pattern of micron crystal glass ceramic film composite material
FIG. 2: containing Lu2BaAl4SiO12:Ce3+Scanning electron image of micron crystal glass ceramic film composite material
FIG. 3: excited by blue laser and contains Lu2BaAl4SiO12:Ce3+Electroluminescent spectrum of micron crystal glass ceramic membrane composite material
FIG. 4: excited by blue laser and contains Lu2BaAl4SiO12:Ce3+Sample luminescent photograph of micron crystal glass ceramic membrane composite material
Detailed Description
Example 1: the target crystal phase in this example was (Lu)2M)(Al4Si)O12:Ce3+Lu of Chinese medicine2BaAl4SiO12:Ce3 +Will analyze pure SiO2；B2O3；Al2O3；Lu2O3；CeO2；BaCO3Powder of 35SiO2-30B2O3-5Al2O3-15Lu2O3-3CeO2-12BaCO3Grinding in agate mortar for more than half an hour to mix uniformly, placing in alumina crucible, placing in 1500 deg.C high temperature furnace, holding for 2 hr, pouring molten glass into copper mold, continuously heat treating at 520 deg.C for 120 min, pulverizing, grinding, and sieving to obtain product containing Lu2BaAl4SiO12:Ce3+Microcrystalline glass ceramic powder. Meanwhile, according to the weight ratio of terpineol: the ethyl cellulose 97 wt% to 3 wt% was weighed and mixed at 80 ℃ under 600 rpm to prepare an organic slurry mixture. Weighing the organic slurry mixture and the low-melting-point glass powder (10 SiO) according to the mass ratio of 1:1:12-35P2O5-24Al2O3-5Na2CO3-26K2CO3Mol%) and Lu-containing2BaAl4SiO12:Ce3+Respectively mixing and grinding the microcrystalline glass ceramic powder in an agate mortar uniformly to obtain coating slurry; then, coating the slurry on a transparent sapphire substrate by a screen printing method, controlling the thickness by the screen printing times, transferring the coated substrate into a 300 ℃ oven, standing for 10 hours for glue removal to fully volatilize an organic mixture in the substrate, and finally sintering the substrate in a 600 ℃ muffle furnace for 20 minutes to obtain the substrate containing Lu2BaAl4SiO12:Ce3+Micron crystal glass ceramic membrane composite material.
X-ray diffraction data show Lu-containing2BaAl4SiO12:Ce3+Except the amorphous peak package presented by the glass substrate, the micron crystal glass ceramic membrane composite material has the position of the crystal phase diffraction peak and Lu2BaAl4SiO12:Ce3+The standard card of (a) corresponds to (b) no clutter signal (as shown in figure 1). Irregular spherical Lu can be seen by scanning electron image of material2BaAl4SiO12:Ce3+The microcrystalline particles are randomly distributed in the glass matrix (as shown in figure 2). Subsequently, using a self-built laser display test system, Lu under blue laser excitation was determined2BaAl4SiO12:Ce3+The electroluminescence spectrum of the micron crystal glass ceramic membrane composite material can effectively generate white light due to the rapid conduction effect of the high-thermal-conductivity transparent sapphire substrate in the composite material on a large amount of heat at a light spot (as shown in figure 3). As shown in FIG. 4, it shows the Lu content under the excitation of blue laser2BaAl4SiO12:Ce3+The luminescent photograph of the sample of the micron crystal glass ceramic membrane composite material shows bright white light. The above data all indicate that the material of the present invention is a novel material that can be used for laser illumination.
Example 2: the target crystal phase in this example was (Lu)2M)(Al4Si)O12:Ce3+Lu of Chinese medicine2(Sr0.5,Ba0.5)Al4SiO12:Ce3+Will analyze pure SiO2；B2O3；Al2O3；Lu2O3；CeO2；SrCO3；BaCO3Powder of 30SiO2-26B2O3-15Al2O3-10.9Lu2O3-0.1CeO2-9SrCO3-9BaCO3Grinding in agate mortar for more than half an hour to mix uniformly, placing in alumina crucible, placing in 1450 deg.C high-temperature furnace, holding for 2 hr, pouring molten glass into copper mold, continuously heat treating at 520 deg.C for 120 min, pulverizing, grinding, and sieving to obtain product containing Lu2(Sr0.5,Ba0.5)Al4SiO12:Ce3+Microcrystalline glass ceramic powder. Meanwhile, according to the weight ratio of terpineol: the ethyl cellulose 97 wt% to 3 wt% was weighed and mixed at 80 ℃ under 600 rpm to prepare an organic slurry mixture. Weighing the organic slurry mixture, the low-melting-point glass powder and the solution containing Lu according to the mass ratio of 1:1:12(Sr0.5,Ba0.5)Al4SiO12:Ce3+Respectively mixing and grinding the microcrystalline glass ceramic powder in an agate mortar uniformly to obtain coating slurry; then, coating the slurry on a transparent sapphire substrate by a screen printing method, controlling the thickness by the screen printing times, transferring the coated substrate into a 300 ℃ oven, standing for 10 hours for glue removal to fully volatilize an organic mixture in the substrate, and finally sintering the substrate in a 550 ℃ muffle furnace for 20 minutes to obtain the product containing Lu2(Sr0.5,Ba0.5)Al4SiO12:Ce3+The micron crystal glass ceramic membrane composite material can be used for laser illumination.
Example 3: the target crystal phase in this example was (Lu)2M)(Al4Si)O12:Ce3+Lu of Chinese medicine2(Ca0.5,Sr0.5)Al4SiO12:Ce3+Will analyze pure SiO2；B2O3；Al2O3；Lu2O3；CeO2；SrCO3；BaCO3Powder of 42SiO2-37B2O3-6Al2O3-5Lu2O3-5CeO2-2.5CaCO3-2.5SrCO3Grinding in agate mortar for more than half an hour to mix uniformly, placing in alumina crucible, placing in 1600 deg.C high-temperature furnace, holding for 2 hr, pouring molten glass into copper mold, continuously heat treating at 520 deg.C for 120 min, pulverizing, grinding, and sieving to obtain product containing Lu2(Ca0.5,Sr0.5)Al4SiO12:Ce3+Microcrystalline glass ceramic powder. Meanwhile, according to the weight ratio of terpineol: the ethyl cellulose is 97 wt% to 3 wt%, and the weight ratio is measured at 80 ℃ and 600And mixing and stirring under the condition of stirring to prepare an organic slurry mixture. Weighing the organic slurry mixture, the low-melting-point glass powder and the solution containing Lu according to the mass ratio of 1:1:12(Ca0.5,Sr0.5)Al4SiO12:Ce3+Respectively mixing and grinding the microcrystalline glass ceramic powder in an agate mortar uniformly to obtain coating slurry; then, coating the slurry on a transparent sapphire substrate by a screen printing method, controlling the thickness by the screen printing times, transferring the coated substrate into a 300 ℃ oven, standing for 10 hours for glue removal to fully volatilize an organic mixture in the substrate, and finally sintering the substrate in a 700 ℃ muffle furnace for 20 minutes to obtain the substrate containing Lu2(Ca0.5,Sr0.5)Al4SiO12:Ce3+The micron crystal glass ceramic membrane composite material can be used for laser illumination.
Example 4: the target crystal phase in this example was (Lu)2M)(Al4Si)O12:Ce3+Lu of Chinese medicine2(Mg0.5,Ca0.5)Al4SiO12:Ce3+Will analyze pure SiO2；B2O3；Al2O3；Lu2O3；CeO2；SrCO3；BaCO3Powder of 30SiO2-26B2O3-15Al2O3-10Lu2O3-5CeO2-7MgCO3-7CaCO3Grinding in agate mortar for more than half an hour to mix uniformly, placing in alumina crucible, placing in 1550 deg.C high-temperature furnace, holding for 2 hr, pouring molten glass into copper mold, continuously heat treating at 520 deg.C for 120 min, pulverizing, grinding, and sieving to obtain product containing Lu2(Mg0.5,Ca0.5)Al4SiO12:Ce3+Microcrystalline glass ceramic powder. Meanwhile, according to the weight ratio of terpineol: the ethyl cellulose 97 wt% to 3 wt% was weighed and mixed at 80 ℃ under 600 rpm to prepare an organic slurry mixture. Weighing the organic slurry mixture, the low-melting-point glass powder and the solution containing Lu according to the mass ratio of 1:1:12(Mg0.5,Ca0.5)Al4SiO12:Ce3+Respectively mixing and grinding the microcrystalline glass ceramic powder in an agate mortar uniformly to obtain coating slurry; then, coating the slurry on a transparent sapphire substrate by a screen printing method, controlling the thickness by the screen printing times, transferring the coated substrate into a 300 ℃ oven, standing for 10 hours for glue removal to fully volatilize an organic mixture in the substrate, and finally sintering the substrate in a 680 ℃ muffle furnace for 20 minutes to obtain the substrate containing Lu2(Mg0.5,Ca0.5)Al4SiO12:Ce3+The micron crystal glass ceramic membrane composite material can be used for laser illumination.

Claims (3)

1. A composite glass-ceramic film is prepared from (Lu)2M)(Al4Si)O12:Ce3+The microcrystalline glass ceramic contains one or more elements selected from Mg, Ca, Sr and Ba as component 10SiO2-35P2O5-24Al2O3-5Na2CO3-26K2CO3The low-melting-point glass and the organic slurry are uniformly mixed and coated on the transparent sapphire substrate, and the composite material can effectively generate white light under the excitation of 455-nanometer high-power blue laser.
2. A method for preparing a glass ceramic membrane composite as claimed in claim 1, characterized in that 30-42 mol% SiO2；26-37mol％B2O3；5-15mol％Al2O3；5-15mol％Lu2O3；0.1-5mol％CeO2；xmol％MgCO3；ymol％CaCO3；zmol％SrCO3；wmol％BaCO3The total mole amount of the above components is 100 mol%, wherein MgCO is3、CaCO3、SrCO3、BaCO3X, y, z, w of (A) are the corresponding target solid solution crystal phases, i.e., (Lu)2M)(Al4Si)O12:Ce3+The solid solution proportion of M is one or more elements selected from Mg, Ca, Sr and Ba, the total mole amount of x + y + z + w is 5-25 mol%, the mixture is evenly ground and then placed in a crucible,placing the mixture into a 1450-2M)(Al4Si)O12:Ce3+Microcrystalline glass ceramic powder, and at the same time, the weight ratio of terpineol: weighing 97 wt% of ethyl cellulose and 3 wt%, mixing and stirring at 80 ℃ and 600 revolutions to prepare an organic slurry mixture, and weighing the organic slurry mixture according to the mass ratio of 1:1:1 to obtain a mixture with the composition of 10SiO2-35P2O5-24Al2O3-5Na2CO3-26K2CO3Low melting point glass powder of (1) and (Lu) containing2M)(Al4Si)O12:Ce3+Respectively mixing and grinding micron crystal glass ceramic powder in an agate mortar to obtain coating slurry, coating the slurry on a transparent sapphire substrate by a screen printing method, controlling the thickness by the number of screen printing, transferring the coated substrate to a 300 ℃ oven, standing for 10 hours for glue removal to fully volatilize the organic mixture, and finally sintering in a 550-700 ℃ muffle furnace for 20 minutes to obtain the product (Lu)2M)(Al4Si)O12:Ce3+Micron crystal glass ceramic membrane composite material.
3. Use of a glass ceramic membrane composite according to claim 1 or a glass ceramic membrane composite produced by the production method according to claim 2, for laser illumination.
CN202110154403.1A 2021-02-04 2021-02-04 Glass ceramic membrane composite material for laser illumination Active CN112851124B (en)

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CN115340366B (en) * 2022-08-12 2024-02-27 江苏师范大学 High-color-rendering-index full-spectrum fluorescent material and preparation method thereof

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