CN116082029A - Preparation method of fluorescent device for reflective laser illumination - Google Patents
Preparation method of fluorescent device for reflective laser illumination Download PDFInfo
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- 238000005286 illumination Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- 239000000919 ceramic Substances 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 239000011521 glass Substances 0.000 claims abstract description 32
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 239000013590 bulk material Substances 0.000 claims description 2
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Abstract
The invention discloses a preparation method of a fluorescent device for reflective laser illumination, which is characterized in that the fluorescent device is prepared according to a chemical formula nAL 2 O 3 ‑(Ce 0.002 Y 0.998 ) 3 Al 5 O 12 The stoichiometric ratio of each element in the powder is more than or equal to 0 and less than or equal to 0.8, namely respectively weighing aluminum oxide, yttrium oxide and cerium oxide, and taking the aluminum oxide, the yttrium oxide and the cerium oxide as raw material powder; sequentially ball milling, drying, sieving, tabletting and sintering in a vacuum sintering furnace at high temperature; the obtained block materialCrushing the materials by adopting a ceramic pair roller machine, and sieving; mixing ceramic powder and glass powder, pouring the mixture into a red copper mold, and placing the red copper mold into a muffle furnace for sintering; cutting the block material, and polishing the surface of the luminescent material to obtain the fluorescent device. The invention provides a fluorescent device sintered on a red copper substrate by mixing and co-firing fluorescent ceramic powder and glass powder; the fluorescent device has excellent overall heat conducting performance, and solves the technical problem of the current fluorescent ceramic package.
Description
Technical Field
The invention relates to the field of laser illumination, in particular to a preparation method of a fluorescent device for reflection type laser illumination.
Background
The laser light source has the remarkable advantages of environmental protection, energy saving, high luminous efficiency, high efficiency, small volume and the like, and is mainly applied to the fields of laser projection, laser flashlight, automobile illumination and the like. The laser illumination light source mainly comprises: fluorescent conversion materials, LD light emitting units, light shaping units, heat sinks, fixed protection units, drivers, and the like. The rare earth light conversion material is used as a core light emitting element, and the performance of the rare earth light conversion material determines the brightness and the system integration level of the illumination light source. Thus, the encapsulation scheme of the luminescent material is a core problem. The "patch-type" packaging mode of phosphor materials and organic resins is limited by low thermal conductivity (typically at 0.5 W.m -1 K -1 ) It is difficult to endure strong thermal shock for a long time, so that temperature quenching, luminescence saturation and even partial carbonization are easily generated. Therefore, the adoption of an inorganic fluorescent conversion material with stronger thermal robustness in combination with excitation packaging mode is a current research hot spot. Such as fluorescent glass, fluorescent ceramics (the heat conductivity of glass is generally 1.0 W.m -1 K -1 The thermal conductivity of the fluorescent ceramic is generally 10 W.m -1 K -1 )。
CN111675489a discloses that the fluorescent powder and the low-melting-point optical glass powder are uniformly mixed, and the glass ceramic fluorescent sheet is prepared through the technological conditions of forming, calcining, cutting, grinding and the like. The material is also fluorescent glass material, and has low heat conduction performance and poor heat stability. CN112174647a discloses the use of inorganic glass phases to sinter fluorescent, light-scattering and highly thermally conductive phases (Al 2 O 3 Etc.) are bonded together to form a ceramic block material. According to the scheme, all the powder is co-fired, and as the decomposition temperature of each powder is uncontrollable, the requirements on an inorganic glass system, a melting point and the like are very high; in addition, the powder bodies are co-fired, and the oxide high-thermal-conductivity phase really plays a role in heat dissipation. CN108527960a discloses a fluorescent ceramic and sapphire composite ceramic material, which comprises a fluorescent ceramic layer, a sapphire layer and a connecting layer, wherein the connecting layer is made of quartz glass, aluminate glass or borate glass. In the scheme, the connecting layer between the high heat conduction substrate (sapphire) and the luminescent material is still made of glass material, so that the heat conduction performance is poor, and the problem of heat effect cannot be effectively solved.
Therefore, it is necessary to design and prepare a fluorescent device with excellent heat dissipation performance, which can resist laser excitation with high power density and ensure stable operation of the luminescent material.
Disclosure of Invention
The invention aims to provide a preparation method of a fluorescent device for reflective laser illumination, and the prepared fluorescent device has excellent heat conduction performance.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of a fluorescent device for reflection type laser illumination comprises the following steps:
(1) According to the chemical formula nAL 2 O 3 -(Ce 0.002 Y 0.998 ) 3 Al 5 O 12 The stoichiometric ratio of each element in the powder is more than or equal to 0 and less than or equal to 0.8, namely respectively weighing aluminum oxide, yttrium oxide and cerium oxide, and taking the aluminum oxide, the yttrium oxide and the cerium oxide as raw material powder;
(2) Sequentially ball milling, drying and sieving the raw material powder in the step (1);
(3) Tabletting the powder sieved in the step (2), and then sintering in a vacuum sintering furnace;
(4) Crushing the block material obtained in the step (3) by adopting a ceramic twin-roll machine, and sieving;
(5) Mixing the ceramic powder obtained in the step (4) with glass powder, pouring the mixture into a red copper mold, and putting the red copper mold into a muffle furnace for sintering;
(6) Cutting the block material obtained by sintering in the step (5), and polishing the surface of the luminescent material to obtain the fluorescent device.
Preferably, in the step (3), the sintering temperature is 1500-1780 ℃ and the sintering time is 5-12 h.
Preferably, in the step (4), the number of the sieved meshes is 10-80 mesh.
Preferably, in the step (5), the mesh number of the glass powder is 200-500 mesh, and the weight ratio of the ceramic powder to the glass powder is 10:1-3:1.
Preferably, in the step (5), the sintering temperature is 400-1000 ℃ and the sintering time is 0.5-1.0 h.
Preferably, in the step (6), the thickness of the polished light-emitting layer of the bulk material is 0.2-1.0 mm.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention mixes and co-burns the fluorescent ceramic powder and the glass powder, prepares the fluorescent ceramic (prepared above 1500 ℃, has the characteristics of high impact resistance, high heat conductivity and the like), and mixes the fluorescent ceramic powder and the glass after crushing and sinters the fluorescent ceramic powder and the glass powder on a red copper substrate. Because the ceramic powder is sintered at a high temperature of more than 1500 ℃, when the ceramic powder is mixed with the glass powder and then sintered for the second time at a temperature of about 1000 ℃, the powder cannot react, so that the packaging scheme of the invention is advanced, the overall heat-conducting performance of the fluorescent device is excellent, and the technical problem of the current fluorescent ceramic package is solved.
2. The invention provides a fluorescent device with better impact resistance and heat conduction performance. The invention provides a ceramic material sintered on a red copper substrate. The fluorescent ceramic has high heat conductivity, and the heat conductivity of the fluorescent ceramic is further improved after the doped alumina is co-fired. The glass powder is introduced in a lower amount, is only used for fixing a sample, and plays a role in heat dissipationThe fluorescent ceramic and red copper materials are used. Compared with a fluorescent device packaged by silica gel and glass, the fluorescent device has better impact performance (20W/mm can be realized 2 ) The heat conduction performance is more excellent (approaching 20.0 W.m -1 K -1 )。
3. The fluorescent device of the invention is 20W/mm 2 Under the excitation of laser, the luminous efficiency is 185-285 lm/W; the operation temperature is 50-165 ℃, the production process is simple, and the method is suitable for industrialization.
Drawings
FIG. 1 is a schematic diagram of a fluorescent conversion device package according to the present invention;
in the figure, 01, a light-emitting layer, 02 and a red copper substrate.
Fig. 2 is a schematic view showing the light emission and heat flow distribution of the fluorescent device of the present invention.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Example 1
A preparation method of a fluorescent material for reflective laser illumination comprises the following steps:
(1) According to the chemical formula (Ce 0.002 Y 0.998 ) 3 Al 5 O 12 Weigh Al 2 O 3 、Y 2 O 3 、CeO 2 Raw material powder, namely pure YAG fluorescent ceramics; wherein Al is 2 O 3 Is 25.751g, Y 2 O 3 34.149g CeO 2 0.104g, and 60.004g.
(2) Ball milling the powder in the step (1) by adopting alcohol as a solvent and alumina balls as ball milling media; ball milling rotating speed is 150r/min, and ball milling time is 24h; then the slurry is put into a baking oven for drying at the temperature of 50 ℃ for 24 hours; then, sieving the dried powder with a 200-mesh screen;
(3) Tabletting the powder obtained in the step (2), and sintering in a vacuum sintering furnace; the sintering temperature is 1780 ℃ and the sintering time is 12 hours;
(4) Crushing the block material obtained in the step (3) by adopting a ceramic twin-roll machine, and sieving with a 80-mesh sieve;
(5) Pouring the ceramic powder and the glass powder obtained in the step (4) into a red copper mold with a groove structure, and then placing the red copper mold into a muffle furnace for sintering at 400 ℃ for 0.5h; wherein the glass powder is 200 meshes of low-melting-point glass powder, and the weight ratio of the ceramic powder to the glass powder is 3:1;
(6) Cutting the block material obtained in the step (5), polishing the surface of the luminescent material, and forming the luminescent layer with the thickness of 1.0mm.
The prepared fluorescent ceramic device is shown in fig. 1. Inside the red copper substrate 02, there is a luminescent layer 01, i.e. a vitrified fluorescent ceramic material. The fluorescent device was tested and placed at 20W/mm as in FIG. 2 2 Under the excitation of laser, the luminous efficiency is 185lm/W; the operating temperature was 165 ℃.
Example 2
A preparation method of a fluorescent material for reflective laser illumination comprises the following steps:
(1) According to chemical formula 0.8Al 2 O 3 -(Ce 0.002 Y 0.998 ) 3 Al 5 O 12 Weigh Al 2 O 3 、Y 2 O 3 、CeO 2 Raw material powder; al (Al) 2 O 3 The weight ratio of the YAG to the Ce is 80 wt%, namely the complex phase-YAG fluorescent ceramic; wherein Al is 2 O 3 Is 40.976g, Y 2 O 3 18.972g CeO 2 0.058g, total 60.006g.
(2) Ball milling the powder in the step (1) by adopting alcohol as a solvent and alumina balls as ball milling media; ball milling rotating speed is 150r/min, and ball milling time is 24h; then the slurry is put into a baking oven for drying at the temperature of 50 ℃ for 24 hours; then, sieving the dried powder with a 200-mesh screen;
(3) Tabletting the powder obtained in the step (2), and sintering in a vacuum sintering furnace; the sintering temperature is 1500 ℃, and the sintering time is 5 hours;
(4) Crushing the block material obtained in the step (3) by adopting a ceramic twin-roll machine, and sieving the block material with a 10-mesh sieve;
(5) Pouring the ceramic powder and the glass powder obtained in the step (4) into a red copper mold with a groove structure, and then placing the red copper mold into a muffle furnace for sintering at the temperature of 1000 ℃ for 1.0h; wherein the glass powder is borosilicate glass with 500 meshes, and the weight ratio of the ceramic powder to the glass powder is 10:1;
(6) Cutting the block material obtained in the step (5), polishing the surface of the luminescent material, and forming a luminescent layer with the thickness of 0.2mm;
the prepared fluorescent ceramic device is shown in fig. 1. Inside the red copper substrate 02, there is a luminescent layer 01, i.e. a vitrified fluorescent ceramic material. The fluorescent device was tested and placed at 20W/mm 2 Under laser excitation, as shown in fig. 2. Its luminous efficiency 222lm/W; the operating temperature was 105 ℃. Compared with example 1, the example has lower operation temperature, mainly because the thermal conductivity of the complex-phase fluorescent ceramic is higher, and the adopted glass powder performance is more excellent (including mesh number and sintering temperature), so that the manufactured fluorescent device has better heat dissipation performance. In addition, this embodiment has higher luminous efficiency than embodiment 1, mainly because the complex phase ceramic has stronger heat radiation to light and higher blue light absorption capability. Meanwhile, better external conditions (namely high heat dissipation performance) ensure the luminous efficiency of the fluorescent device.
Example 3
A preparation method of a fluorescent material for reflective laser illumination comprises the following steps:
(1) According to chemical formula 0.6Al 2 O 3 -(Ce 0.002 Y 0.998 ) 3 Al 5 O 12 Weigh Al 2 O 3 、Y 2 O 3 、CeO 2 Raw material powder; al (Al) 2 O 3 The weight ratio of the YAG to the Ce is 60wt percent, namely the complex phase-YAG fluorescent ceramic; wherein Al is 2 O 3 Is 38.594g, Y 2 O 3 21.343g CeO 2 0.065g, 60.002g total;
(2) Ball milling the powder in the step (1) by adopting alcohol as a solvent and alumina balls as ball milling media; ball milling rotating speed is 150r/min, and ball milling time is 24h; then the slurry is put into a baking oven for drying at the temperature of 50 ℃ for 24 hours; then, sieving the dried powder with a 200-mesh screen;
(3) Tabletting the powder obtained in the step (2), and sintering in a vacuum sintering furnace; sintering temperature is 1650 ℃ and sintering time is 5h;
(4) Crushing the block material obtained in the step (3) by adopting a ceramic twin-roll machine, and sieving the block material with a 10-mesh sieve;
(5) Pouring the ceramic powder and the glass powder obtained in the step (4) into a red copper mold with a groove structure, and then placing the red copper mold into a muffle furnace for sintering at the temperature of 1000 ℃ for 1.0h; wherein the glass powder is borosilicate glass with 300 meshes, and the weight ratio of the ceramic powder to the glass powder is 10:1;
(6) Cutting the block material obtained in the step (5), polishing the surface of the luminescent material, and forming a luminescent layer with the thickness of 0.2mm;
the prepared fluorescent ceramic device is shown in fig. 1. Inside the red copper substrate 02, there is a luminescent layer 01, i.e. a vitrified fluorescent ceramic material. The fluorescent device was tested and placed at 20W/mm 2 Under laser excitation, as shown in fig. 2. The luminous efficiency is 285lm/W; the operating temperature was 50 ℃. Compared with the embodiment 2, the embodiment has lower operation temperature mainly because the sintering temperature of the fluorescent ceramic is higher, the heat preservation time is longer, the internal air holes are obviously reduced, and the density and the heat conductivity of the complex-phase ceramic are improved, so that the manufactured fluorescent device has better heat dissipation performance. In addition, this embodiment has higher luminous efficiency than embodiment 2, mainly because the content of luminescent ions is higher, the amount of absorbed blue light is larger, and the generated fluorescence is stronger in the fluorescent device, and thus the luminous efficiency is higher. Meanwhile, better external conditions (namely high heat dissipation performance) ensure the luminous efficiency of the fluorescent device.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.
Claims (6)
1. The preparation method of the fluorescent device for the reflective laser illumination is characterized by comprising the following steps of:
(1) According to the chemical formula nAL 2 O 3 -(Ce 0.002 Y 0.998 ) 3 Al 5 O 12 The stoichiometric ratio of each element in the powder is more than or equal to 0 and less than or equal to 0.8, namely respectively weighing aluminum oxide, yttrium oxide and cerium oxide, and taking the aluminum oxide, the yttrium oxide and the cerium oxide as raw material powder;
(2) Sequentially ball milling, drying and sieving the raw material powder in the step (1);
(3) Tabletting the powder sieved in the step (2), and then sintering in a vacuum sintering furnace;
(4) Crushing the block material obtained in the step (3) by adopting a ceramic twin-roll machine, and sieving;
(5) Mixing the ceramic powder obtained in the step (4) with glass powder, pouring the mixture into a red copper mold, and putting the red copper mold into a muffle furnace for sintering;
(6) Cutting the block material obtained by sintering in the step (5), and polishing the surface of the luminescent material to obtain the fluorescent device.
2. The method of manufacturing a reflective laser light emitting phosphor according to claim 1, wherein in the step (3), the sintering temperature is 1500 to 1780 ℃ and the sintering time is 5 to 12 hours.
3. The method of producing a fluorescent device for reflection type laser light illumination of claim 1, wherein in the step (4), the number of the screen meshes of the screen is 10 to 80 mesh.
4. The method of manufacturing a reflective laser light emitting phosphor according to claim 1, wherein in the step (5), the mesh number of the glass frit is 200 to 500 mesh, and the weight ratio of the ceramic powder to the glass frit is 10:1 to 3:1.
5. The method of manufacturing a reflective laser light emitting phosphor according to claim 1, wherein in the step (5), the sintering temperature is 400 to 1000 ℃ and the sintering time is 0.5 to 1.0h.
6. The method of manufacturing a reflective laser light emitting phosphor according to claim 1, wherein in the step (6), the thickness of the polished light emitting layer of the bulk material is 0.2 to 1.0mm.
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