CN113024242A - Superfine ceramic phosphor for obtaining high lumen laser illumination and preparation method thereof - Google Patents
Superfine ceramic phosphor for obtaining high lumen laser illumination and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 46
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000005286 illumination Methods 0.000 title claims description 19
- 238000002360 preparation method Methods 0.000 title claims description 9
- 230000005284 excitation Effects 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 7
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- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 3
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052593 corundum Inorganic materials 0.000 claims description 9
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- 235000015895 biscuits Nutrition 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
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Abstract
The invention discloses an ultra-fine ceramic phosphor for obtaining high lumen laser lighting, the chemical composition of the ceramic phosphor is (Ce)xReyY1‑x‑y)3Al5O12Re is one or more of Lu, Tb, Gd and Ga, wherein the value ranges of x and y are as follows: x is more than or equal to 0.005 and less than or equal to 0.05, and y is more than or equal to 0 and less than or equal to 0.25; the ceramic phosphor is prepared by a self-assembly complex phase method. The invention has the beneficial effects that: has excellent luminous efficiency and stability, and the luminous flux can be obtained under the excitation of a single laser module (8 blue lasers are converged)Reaching more than 3 klm and meeting the application of high lumen laser lighting.
Description
Technical Field
The invention relates to a superfine ceramic phosphor for obtaining high lumen laser illumination and a preparation method thereof.
Background
The microstructure of the material has an important influence on the luminescence performance, so that the superfine luminescent material, especially the nanometer luminescent material, is the key point of research work in the scientific field. Because the surface of the nano-particles and the interface effect obstruct the energy resonance transmission, the probability of transmitting the excitation energy from the luminescence center to the quenching center is reduced, thereby obviously enhancing the luminescence intensity of the material; and the spin forbidden ring in the energy level relaxation of the luminescent ions is further removed due to the quantum size effect, so that the radiation transition probability is improved or the radiationless relaxation is enhanced, and the luminous efficiency is improved. Therefore, the preparation and research of nano or near-nano fluorescent materials have very positive significance, and no matter the fluorescent materials are used as laser or LED light conversion fluorescent materials, urgent needs are provided for the size of ultra-fine grains at present.
Researchers find that the ultrafine spherical particles with uniform particle size distribution can effectively reduce the independent sedimentation of powder particles in the packaging process and are beneficial to improving the yield of products in the actual use process of the fluorescent powder for LEDs. Meanwhile, with the new Mini LED and Micro LED technologies, research on ultra-fine and high-brightness fluorescent powder is focused. The grain size of the conventional fluorescent powder on the market is 10-20 mu m at present; the superfine fluorescent powder prepared by a sol-gel method, a combustion method, a hydrothermal method, a homogeneous precipitation method and the like has high technical difficulty and high equipment requirement, and is not suitable for large-scale production, for example, the Beijing nonferrous metals institute has developed the superfine fluorescent powder prepared by the combustion method in the patent No. ZL200610058730.2 of the New rare earth materials GmbH; the superfine fluorescent powder obtained by physically crushing the fluorescent powder has low light efficiency and poor thermal stability due to a plurality of surface defects, for example, the superfine fluorescent powder prepared by grinding and crushing method is adopted in the patent with the publication number of 104130778B by Yixing Yimao fluorescent material Limited company; the preparation method of patent No. CN109486490A applied by Jiangsu Borui photoelectricity limited company is relatively simple, and the particle size of the superfine phosphor prepared by adopting the cosolvent combined with the high temperature reduction method is also reduced to 5-7 μm.
However, in high lumen laser illumination applications, multiple laser focusing is typically employed for laser illumination (single laser light power density of about 1.5W/mm)2) The fluorescent material needs to bear much higher power density of blue light irradiation than that of a white light LED, so that compared with fluorescent powder with the phenomenon of 'efficiency dip', YAG-based fluorescent ceramic with the characteristics of high uniformity, high thermal conductivity and thermal aging resistance becomes a preferable research object for laser illumination. Compared with fluorescent powder, YAG-based fluorescent ceramic needs to further undergo a high-temperature densification stage in the preparation process, powder crystal grains grow up in the high-temperature stage, and the fluorescent ceramic with an ultra-fine crystal grain structure is more difficult to obtain.
The laser white light technology is still in the starting stage at present, and the white light LED illumination technology is far from mature. Laser lighting has huge application potential due to the advantages of high energy efficiency, small volume and the like, and is successfully and commercially applied to laser lighting of vehicle lamps at present, but the adopted fluorescent material is mainly resin-encapsulated fluorescent powder, the key technology of the superfine ceramic fluorescent body for high-lumen laser lighting is not mature, and the research and development of fluorescent ceramics and experimental verification and research work are required to be carried out so as to meet the requirement of realizing large-scale application and popularization of laser lighting.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a novel superfine ceramic phosphor for obtaining high-lumen laser illumination and a preparation method thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows: an ultra-fine ceramic phosphor for obtaining high lumen laser lighting, said ceramic phosphor having a chemical composition of (Ce)xReyY1-x-y)3Al5O12Re is one or more of Lu, Tb, Gd and Ga,wherein, the value ranges of x and y are as follows: x is more than or equal to 0.005 and less than or equal to 0.05, and y is more than or equal to 0 and less than or equal to 0.25; the ceramic phosphor is prepared by a self-assembly complex phase method.
As a preferable mode of obtaining the ultrafine ceramic phosphor for high lumen laser lighting, the ceramic phosphor has a crystal structure of YAG phase and Al phase2O3A phase complex structure of, wherein, Al2O3The weight proportion of the phase is 0-60%.
As a preferable scheme of the ultrafine ceramic phosphor for obtaining high lumen laser illumination, the excitation wavelength range of the ceramic phosphor is 420-500nm, and the emission wavelength range formed under the excitation of the excitation light is 450-750 nm.
As a preferable scheme for obtaining the superfine ceramic fluorescent body for high lumen laser illumination, a BLUE PASS antireflection film is attached to the upper surface of the ceramic fluorescent body, and a metal reflecting layer is attached to the lower surface of the ceramic fluorescent body and welded in a copper heat dissipation base.
The invention also provides a preparation method of the superfine ceramic phosphor for obtaining high lumen laser illumination, which is used for preparing the ceramic phosphor and comprises the following steps,
step S1, according to the chemical composition, (Ce)xReyY1-x-y)3Al5O12The metering ratio of the catalyst is prepared by a self-assembly complex phase method;
step S2, mixing (Ce)xReyY1-x-y)3Al5O12Phosphor and Al2O3Mixing the particles with a certain amount of dispersant, epoxy resin and curing agent, stirring and dispersing to obtain uniform aqueous slurry, removing bubbles from the aqueous slurry in vacuum, and performing tape casting to obtain a fluorescent body blank; and the number of the first and second groups,
and step S3, sintering the biscuit at high temperature to obtain the superfine ceramic phosphor.
Said (Ce)xReyY1-x-y)3Al5O12The grain diameter of the fluorescent powder is 100-400nm, and the Al2O3The grain size of the superfine powder is 50-200 nm.
Compared with the prior art, the invention has the beneficial effects that: the high-power laser module has excellent luminous efficiency and stability, and under the excitation of a single laser module (8 blue lasers are converged), luminous flux can reach more than 3 klm, and the high-power laser module meets the application of high-lumen laser illumination.
Drawings
FIG. 1 is a scanning electron micrograph of the cross section of the ultrafine ceramic phosphor of the present invention, in which the YAG phase grain size is in the range of 1-3 μm and Al is present2O3The phase particle size is 1-2 μm.
FIG. 2 shows the luminous flux test of the present invention with the ultra-fine ceramic phosphor as the main body, wherein the luminous flux is not less than 3 klm under the excitation of a single laser module (8 blue lasers are converged).
Detailed Description
The invention will be described in further detail below with reference to specific embodiments and drawings. Here, the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1:
with Y2O3、CeO2And Al (NO)3)3•9H2Preparing nitrate solution with pH value of 3-4 with nitric acid, dissolving Citric Acid (CA) in the nitrate solution as metal ion complexing agent according to (Ce)0.05Y0.95)3Al5O12The fluorescent ceramic is mixed and stirred according to the chemical proportion to obtain transparent solution. Transferring the mixed transparent solution into a Teflon lining reaction kettle, preserving the temperature at 150 ℃ for more than 6h, and self-assembling to synthesize the fluorescent powder with the particle size of 100-500 nm. Mixing the fluorescent powder with commercial nano Al2O3Mixing powder (with particle size of 50 nm) at a ratio of 60% to 40%, adding a certain amount of dispersant, epoxy resin and curing agent, stirring and dispersing to obtain uniform aqueous slurry, removing bubbles from the aqueous slurry under vacuum, and performing tape casting to obtain a fluorescent body blank; sintering the biscuit at high temperature to obtain the finished productThe density of the superfine ceramic phosphor reaches more than 95 percent, and the grain size is 1-3 mu m.
The upper surface and the lower surface of the superfine ceramic phosphor Ce: YAG are respectively plated with a blue light antireflection film and a metal reflection film and are welded in a copper heat dissipation base. A bank with 8 LD (single rated power is 4W) is used as a blue light excitation light source, and the blue light excites the phosphor to emit yellow light, so that stable high-lumen laser illumination is obtained, and the luminous flux is 3.688 klm (@ 2.4A current).
Example 2:
with Y2O3、CeO2And Al (NO)3)3•9H2Preparing nitrate solution with pH value of 3-4 with nitric acid, dissolving Citric Acid (CA) in the nitrate solution as metal ion complexing agent according to (Ce)0.08Y0.92)3Al5O12The fluorescent ceramic is mixed and stirred according to the chemical proportion to obtain transparent solution. Transferring the mixed transparent solution into a Teflon lining reaction kettle, preserving the temperature at 150 ℃ for more than 6h, and self-assembling to synthesize the fluorescent powder with the particle size of 100-500 nm. Mixing the fluorescent powder with commercial nano Al2O3The powder (with the particle size of 50 nm) is proportioned according to the mass ratio of 70% to 30%, then a certain amount of dispersant, epoxy resin and curing agent are added, uniform aqueous slurry is obtained by stirring and dispersing, and then the aqueous slurry is subjected to casting after vacuum defoaming, so as to obtain a fluorescent body biscuit; and sintering the biscuit at high temperature to obtain the superfine ceramic phosphor with the density of more than 95 percent, wherein the grain size is 1-3 mu m.
The upper surface and the lower surface of the superfine ceramic phosphor Ce: YAG are respectively plated with a blue light antireflection film and a reflecting film and are welded in a copper heat dissipation base. A bank with 8 LD (rated power of 4W and 32W) is used as a blue light excitation light source, and the blue light excitation phosphor emits yellow light, so that stable high-lumen laser white light illumination is obtained, and the luminous flux is 3.711 klm (@ 2.4A current).
The foregoing merely represents embodiments of the present invention, which are described in some detail and detail, and therefore should not be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. An ultrafine ceramic phosphor for obtaining high lumen laser illumination, characterized in that the chemical composition of the ceramic phosphor is (Ce)xReyY1-x-y)3Al5O12Re is one or more of Lu, Tb, Gd and Ga, wherein the value ranges of x and y are as follows: x is more than or equal to 0.005 and less than or equal to 0.05, and y is more than or equal to 0 and less than or equal to 0.25; the ceramic phosphor is prepared by a self-assembly complex phase method.
2. The ultra-fine ceramic phosphor for obtaining high lumen laser illumination of claim 1, wherein the crystal structure of said ceramic phosphor is YAG phase and Al2O3A phase complex structure of, wherein, Al2O3The weight proportion of the phase is 0-60%.
3. The ultra-fine ceramic phosphor for obtaining high lumen laser illumination as claimed in claim 1, wherein the excitation wavelength range of the ceramic phosphor is 420-500nm, and the wavelength range of the emitted light formed under the excitation of the excitation light is 450-750 nm.
4. The method of claim 1, wherein a BLUE PASS anti-reflection film is attached to the upper surface of the ceramic phosphor, and a metal reflective layer is attached to the lower surface of the ceramic phosphor and soldered in a copper heat dissipation base.
5. A method for preparing an ultrafine ceramic phosphor for obtaining high lumen laser illumination for use in the preparation of a ceramic phosphor according to any one of claims 1 to 4, characterized by comprising the steps of,
step S1, according to the chemical composition, (Ce)xReyY1-x-y)3Al5O12The metering ratio of the catalyst is prepared by a self-assembly complex phase method;
step S2, mixing (Ce)xReyY1-x-y)3Al5O12Phosphor and Al2O3Mixing the particles with a certain amount of dispersant, epoxy resin and curing agent, stirring and dispersing to obtain uniform aqueous slurry, removing bubbles from the aqueous slurry in vacuum, and performing tape casting to obtain a fluorescent body blank; and the number of the first and second groups,
and step S3, sintering the biscuit at high temperature to obtain the superfine ceramic phosphor.
6. The method for preparing the ultrafine ceramic phosphor for obtaining high lumen laser illumination according to claim 4, wherein the (Ce) isxReyY1-x-y)3Al5O12The grain diameter of the fluorescent powder is 100-400nm, and the Al2O3The grain size of the superfine powder is 50-200 nm.
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