CN116217218A - Fluorescent ceramic with composite structure and preparation method thereof - Google Patents
Fluorescent ceramic with composite structure and preparation method thereof Download PDFInfo
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- CN116217218A CN116217218A CN202211506084.7A CN202211506084A CN116217218A CN 116217218 A CN116217218 A CN 116217218A CN 202211506084 A CN202211506084 A CN 202211506084A CN 116217218 A CN116217218 A CN 116217218A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 121
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims abstract description 49
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 40
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 235000015895 biscuits Nutrition 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005520 cutting process Methods 0.000 claims abstract description 13
- 238000003825 pressing Methods 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000009694 cold isostatic pressing Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 7
- 238000005056 compaction Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims 10
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 claims 10
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 17
- 230000017525 heat dissipation Effects 0.000 abstract description 10
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 229920006395 saturated elastomer Polymers 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 10
- 238000005286 illumination Methods 0.000 description 10
- 239000011521 glass Substances 0.000 description 8
- 230000005284 excitation Effects 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
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- F21V13/04—Combinations of only two kinds of elements the elements being reflectors and refractors
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Abstract
The invention discloses a fluorescent ceramic with a composite structure and a preparation method thereof, and relates to the technical field of luminescent materials. The fluorescent ceramic with the composite structure comprises Al which is arranged up and down 2 O 3 YAG-Ce complex phase ceramic, YAG transparent ceramic and Al with edge 2 O 3 A ceramic; al is added with 2 O 3 Mixing and pressing the raw materials of the YAG-Ce and YAG ceramics respectivelyPreparing a biscuit, sintering, preserving heat and cutting the biscuit to obtain chip-level Al 2 O 3 -YAG: ce/YAG composite fluorescent ceramic; al is added with 2 O 3 Pressing the powder and the chip-level composite fluorescent ceramic into a biscuit, and sintering and preserving heat to obtain Al 2 O 3 ‑YAG:Ce/YAG/Al 2 O 3 Fluorescent ceramics with composite structure. The fluorescent ceramic designed by the invention has high luminous efficiency, good heat dissipation performance and high saturated power density, and is suitable for a transmission type laser lighting system; in addition, the annealing process of the fluorescent ceramic and the sintering process of the alumina ceramic are combined into a whole, and the preparation process is simple and suitable for industrialization.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a fluorescent ceramic with a composite structure and a preparation method thereof.
Background
The laser illumination has the excellent characteristics of high power, high brightness, high collimation and the like, and has great application potential in the new technical aspects of automobile headlamps, airport illumination, searchlight, projection and the like. Laser illumination techniques generally include reflective illumination structures and transmissive illumination structures. The most typical application of the reflective mechanism is a laser projector, which is usually composed of a collimated blue Laser Diode (LD) remotely excited yellow luminescent material. These yellow luminescent materials are required to have opaque, highly reflective properties to increase their light extraction efficiency; in addition, to ensure stable operation, the yellow luminescent material is encapsulated on the copper substrate by solder. The reflective illumination structure can obtain high brightness; however, the reflective structure exposes many problems such as complicated beam shaping, poor illumination uniformity, and large volume due to the non-uniformity of the paths between the blue laser and the yellow fluorescent light.
In contrast, in the transmissive structure, the transmission direction of the blue laser light coincides with the fluorescence direction, which makes it a main structural form of laser illumination. Fluorescent materials used in transmission typically include silica gel encapsulated phosphors, fluorescent glasses, and fluorescent ceramics. As is well known, the thermal conductivity of the phosphor powder packaged by silica gel is the lowest, generally 0.1 to the whole0.4W·m -1 ·K -1 This causes thermal focusing at the laser spot, resulting in an excessively high operating temperature. In addition, silica gels are easily carbonized (over 150 ℃) under high power density laser excitation. Therefore, fluorescent glass and fluorescent ceramics are the main research materials. The fluorescent glass is made of transparent glass and fluorescent powder, the preparation process is very simple, and chromaticity parameters (including CCT and CRI) are very convenient to tune by selecting different fluorescent powder. However, its thermal conductivity is not very high (1.0-3.0 W.m -1 ·K -1 ) Cannot bear high power (more than or equal to 5.0W) and high density (more than or equal to 10W/mm) 2 ) Is a laser excitation of (c). The fluorescent ceramic has higher thermal stability and thermal conductivity (9.0-14.0 W.m) -1 ·K -1 ) Becomes an ideal choice for high-power laser illumination.
In addition to the requirement of the luminescent material for high thermal conductivity, an excellent optical system and an excellent heat dissipation system are also indispensable in the transmissive structure. First, because of the high collimation of the laser beam, fluorescent ceramics are typically made translucent and used for light scattering. That is, the second phase serves as a scattering center, reduces the transmittance of the fluorescent ceramic, and changes the propagation direction of blue light to obtain more efficient and uniform white light. In addition, the second relative thermal stability improvement is of great benefit, such as Al 2 O 3 (32～35W m -1 K -1 )、MgO(47.2～53.5W m -1 K -1 )、AlN(320W m -1 K -1 ) The high thermal conductivity is beneficial to improving the heat dissipation capacity of the fluorescent ceramics. Second, the size of the fluorescent ceramic is typically in the order of millimeters for controlling the spot diameter of the white light source. Finally, the encapsulation material should have high transparency and high thermal conductivity and have no effect on the absorption and emission of the luminescent material.
However, most solders and other joining materials commonly used in reflective structures are opaque and cannot be used in transmissive structures. Expert students can only develop other designs: for example, paper Co-sintered ceramic converter for transmissivelaser-activated remote phosphor conversion, the foreign Lenef team designed a new structure, al 2 O 3 Porous ceramicCo-firing with complex phase ceramics (Al 2 O 3 -YAG:Ce/Al 2 O 3 ). By placing the complex phase ceramic at highly scattering Al 2 O 3 In the substrate (simply understood as a "taping mechanism"), the co-sintered ceramic can be stably operated under 4.3W laser excitation. The luminous flux is 600lm at the most, and the corresponding peak brightness is 500cd/mm 2 . The packaging method can be used for chip-scale ceramic
And performing effective encapsulation. However, the film is limited by heat-induced light attenuation, and only 150lm/W is adopted after film coating. This is mainly due to the fact that the bottom of the luminescent material is to ensure blue laser incidence, al cannot be used 2 O 3 Encapsulation of the porous material results in only the ceramic at the edges being Al 2 O 3 The bottom of the fluorescent ceramic is in a suspended state, so that the effective area for heat dissipation is severely limited. In addition, sapphire is considered as the optimal substrate material for luminescent materials due to its high thermal conductivity, high transparency (-86%) characteristics. Xie et al (paper Unique Color Converter Architecture Enabling Phosphor-in-Glass (PiG) Films Suitable for High-Power and High-Luminance Laser-Driven White Lighting) developed a structure to sinter fluorescent Glass thin films directly onto High thermal conductivity sapphire substrates. The fluorescent glass film can be 11.2W mm 2 Stable luminescence under laser, and high luminous efficiency up to 210lm/W. However, it is difficult for the fluorescent ceramics to be bonded with sapphire. This is mainly due to the difficulty of thermal bonding between the fluorescent ceramic and the sapphire and the difference in sintering conditions, which has not been reported so far. Some scholars use glass frit as a connecting material of the two, but this would not be a problem in reducing heat dissipation. Therefore, a transparent material having high thermal conductivity must be searched for to encapsulate the luminescent ceramic and to compensate for the defects of the laser illumination optical system and the heat dissipation system.
Disclosure of Invention
In view of the above, the invention discloses a fluorescent ceramic with a composite structure and a preparation method thereof, wherein YAG ceramic with high transparency and high thermal conductivity is used as a base material, the heat dissipation area is greatly increased, the heat dissipation performance is more excellent, and the blue light excitation with higher power density can be born.
According to the invention, the fluorescent ceramic with a composite structure comprises Al arranged up and down 2 O 3 YAG-Ce complex phase ceramic, YAG transparent ceramic and Al with edge 2 O 3 And (3) ceramics.
The invention further discloses a preparation method of the fluorescent ceramic with the composite structure, which comprises the following steps:
step one: preparation of Al 2 O 3 -YAG: ce/YAG composite fluorescent ceramic;
s1-1, proportioning: according to Al 2 O 3 The stoichiometric ratio of each element in Ce is respectively calculated by the weight of aluminum oxide, yttrium oxide and cerium oxide; respectively weighing aluminum oxide and yttrium oxide according to the stoichiometric ratio of each element in YAG;
s1-2, ball milling: mixing two groups of raw material powder respectively by taking alumina balls as a medium and alcohol as a solvent;
s1-3, sieving: drying and sieving the mixed powder;
s1-4, tabletting: adopting a dry press to press and mold YAG powder; subsequently Al is added 2 O 3 Pouring YAG Ce powder into a grinding tool for secondary pressing;
s1-5, cold isostatic pressing: compacting the pressed biscuit by adopting a cold extruder;
s1-6, vacuum sintering: placing the compacted biscuit into a vacuum sintering furnace, and sintering the biscuit;
s1-7, cutting: cutting the sintered ceramic by using a cutting machine;
step two: preparing a fluorescent ceramic device with a composite structure;
s2-1, tabletting: adopting a dry press to perform Al 2 O 3 Compacting and forming the powder; then, the obtained biscuit and the ceramic square sheet obtained in the step S1-7 are pressed and formed again;
s2-2, cold isostatic pressing: compacting the pressed biscuit by adopting a cold extruder;
s2-3, sintering and annealing: placing the compacted biscuit into a muffle furnace for sintering;
s2-4, washing, grinding and polishing: surface treatment is carried out by a milling machine and a polishing machine to obtain Al 2 O 3 -YAG:Ce/YAG/Al 2 O 3 Fluorescent ceramics with composite structure.
Preferably, in S1-1, al 2 O 3 YAG-Al in Ce 2 O 3 The mass ratio is 10.0-40.0 wt.%, and the Ce doping degree is 0.2-1.0 at.%.
Preferably, in S1-2, the ball milling time is 24 hours, and the rotating speed is 140-170 r/min.
Preferably, in S1-3, the drying temperature is 55 ℃, and the drying time is 15-20 hours; the number of the screening meshes is 100-200 meshes.
Preferably, in S1-4, the dry press presses YAG powder for the first time under the pressure of 3MPa for 1-5 min; the secondary pressing pressure is 10Mpa, and the pressure maintaining time is 1-5 min; in S1-5, the compaction pressure of the cold extruder is 200Mpa, and the dwell time is 10-15 min.
Preferably, in S1-6, the sintering temperature is 1740-1770 ℃ and the heat preservation time is 12h; in S2-3, the sintering temperature is 1350-1450 ℃ and the sintering time is 12h.
Preferably, the process is carried out in steps S1-7, al 2 O 3 The thickness of the Ce composite ceramic layer is 0.1-0.3 mm, the thickness of the YAG transparent ceramic layer is 0.1-0.3 mm, the side length of the cut ceramic square sheet is 1.0 x 1.0mm, and the thickness is 0.2-0.6 mm.
Preferably, in S2-1, the dry press is specific to Al 2 O 3 The powder pressing pressure is 3Mpa, and the pressure maintaining time is 1-5 min; the pressure of the secondary compression molding is 10Mpa, and the pressure maintaining time is 1-5 min; in S2-2, the compaction pressure of the cold extruder is 200Mpa, and the dwell time is 10-15 min.
Preferably, al is obtained by the steps S2-4 2 O 3 The thickness of the ceramic is 0.2-0.6 mm, al 2 O 3 The thickness of the Ce complex phase ceramic layer is 0.1-0.3 mm, and the thickness of the YAG transparent ceramic layer is 0.1-0.3 mm; the diameter of the fluorescent ceramic with the composite structure is 16.0-20.0 mm, and the thickness is 0.2-0.6 mm.
Compared with the prior art, the fluorescent ceramic with the composite structure and the preparation method thereof have the advantages that:
(1) Compared with a fluorescent ceramic material with a single-pure aluminum oxide or aluminum substrate edge-wrapping structure, the YAG ceramic material with high transparency and high thermal conductivity is adopted as a base material, so that the heat dissipation area is greatly increased, the heat dissipation performance is more excellent, and the blue light excitation with higher power density can be born.
(2) The invention can maintain high luminous efficiency of the complex phase ceramic and high transmittance of the transparent ceramic YAG by controlling the sintering temperature of co-firing.
(3) The invention uses Al 2 O 3 Annealing process and edge-wrapping structure Al of YAG-Ce/YAG composite fluorescent ceramic 2 O 3 The sintering process is integrated, the preparation process is simple, and the method is suitable for industrialization.
Drawings
For a clearer description of embodiments of the invention or of the prior art, the drawings which are used in the description of the embodiments or of the prior art will be briefly described, it being evident that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a fluorescent ceramic of composite structure according to the present disclosure.
Fig. 2 is a system light path diagram of the present invention.
In the figure: 1-Al 2 O 3 -YAG: ce complex phase ceramic; 2-YAG transparent ceramics; 3-Al 2 O 3 A ceramic; 4-film layer.
Detailed Description
The following is a brief description of embodiments of the present invention with reference to the accompanying drawings. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that all other embodiments obtained by a person having ordinary skill in the art without making creative efforts based on the embodiments in the present invention are within the protection scope of the present invention.
Fig. 1-2 illustrate a preferred embodiment of the present invention, which is described in detail.
Example 1
A fluorescent ceramic with a composite structure shown in FIG. 1 comprises Al arranged up and down 2 O 3 YAG, ce composite ceramic 1 and YAG transparent ceramic 2, and Al with edges 2 O 3 And (3) ceramics. The bottom surface of the fluorescent ceramic with the composite structure is also provided with a film layer 4, the transmittance of the film layer 4 at 450nm is 95%, and the reflectivity at 500-800 nm is 95%.
The method for preparing the fluorescent ceramic with the composite structure comprises the following steps:
step one: preparation of Al 2 O 3 YAG, ce/YAG composite fluorescent ceramic.
S1-1, proportioning: according to Al 2 O 3 The stoichiometric ratio of each element in the YAG to Ce is respectively calculated by the weight of aluminum oxide, yttrium oxide and cerium oxide, al 2 O 3 The mass ratio was 40.0wt.%, and the Ce doping level was 1.0at.%. Alumina and yttrium oxide are respectively weighed according to the stoichiometric ratio of each element in YAG.
S1-2, ball milling: the method comprises the steps of respectively mixing two groups of raw material powder by taking alumina balls as a medium and alcohol as a solvent, wherein the ball milling time is 24 hours, and the rotating speed is 140r/min.
S1-3, sieving: and (3) drying and sieving the mixed powder, wherein the drying temperature is 55 ℃, the drying time is 15 hours, and the sieving number is 100 meshes.
S1-4, tabletting: firstly, carrying out compression molding on YAG powder by adopting a dry press, wherein the pressure is 3MPa, and the pressure maintaining time is 1min; subsequently Al is added 2 O 3 YAG, ce powder is poured into a grinding tool to be pressed for the second time, the pressure is 10Mpa, and the pressure maintaining time is 1min.
S1-5, cold isostatic pressing: further compacting the pressed biscuit by adopting a cold extruder, wherein the pressure is 200Mpa, and the pressure maintaining time is 10min.
S1-6, vacuum sintering: and (3) putting the compacted biscuit into a vacuum sintering furnace, sintering the biscuit at 1740 ℃ for 12 hours.
S1-7, cutting: cutting the sintered ceramic by using a cutting machine, wherein the cut ceramic square sheetA side length of 1.0 x 1.0mm and a thickness of 0.2mm, wherein Al 2 O 3 YAG, ce composite ceramic 1 layer with thickness of 0.1mm and YAG transparent ceramic 2 layer with thickness of 0.1mm.
Step two: and preparing the fluorescent ceramic device with the composite structure.
S2-1, tabletting: adopting a dry press to perform Al 2 O 3 The powder is pressed and molded, the pressure is 3Mpa, and the pressure maintaining time is 1min; and then, the obtained biscuit and the ceramic square sheet obtained in the step S1-7 are pressed and molded again, the pressure is 10Mpa, and the pressure maintaining time is 1min.
S2-2, cold isostatic pressing: compacting the pressed biscuit by adopting a cold extruder; the compaction pressure of the cold extruder is 200Mpa and the dwell time is 10min.
S2-3, sintering and annealing: placing the compacted biscuit into a muffle furnace for sintering; the sintering temperature is 1350 ℃ and the sintering time is 12h.
S2-4, washing, grinding and polishing: surface treatment is carried out by a milling machine and a polishing machine to obtain Al 2 O 3 -YAG:Ce/YAG/Al 2 O 3 The diameter of the fluorescent ceramic with the composite structure is 16.0mm, and the thickness is 0.2mm. Wherein Al is 2 O 3 The thickness of the ceramic 3 is 0.2mm, al 2 O 3 YAG, ce composite ceramic 1 layer with thickness of 0.1mm and YAG transparent ceramic 2 layer with thickness of 0.1mm.
As shown in FIG. 2, blue light passes through the film layer 4 and YAG transparent ceramic 2 to excite Al 2 O 3 YAG-Ce complex phase ceramic 1, wherein part of generated fluorescence is emitted from the surface, part of the fluorescence is emitted downwards and is reflected back to the front direction, and the other part of the fluorescence is emitted to the periphery and passes through Al 2 O 3 The scattering of the ceramic 3 is returned to the forward direction. Laser testing is carried out on the fluorescent ceramic device with the composite structure, and when the laser power density is from 1.0W/mm to 60W/mm 2 The luminescence of the ceramic does not appear to be saturated. The surface temperature of the fluorescent ceramic device with the composite structure is increased from 25 ℃ to 99 ℃, and the luminous efficiency is reduced from 182lm/W to 167.7lm/W.
Example 2
A fluorescent ceramic with a composite structure shown in FIG. 1 comprises Al arranged up and down 2 O 3 YAG-Ce complex phase ceramic 1 and YAG transparent ceramic 2 and Al with edge coating 2 O 3 And (3) ceramics. The bottom surface of the fluorescent ceramic with the composite structure is also provided with a film layer 4, the transmittance of the film layer 4 at 450nm is 99%, and the reflectivity at 500-800 nm is 99%.
The method for preparing the fluorescent ceramic with the composite structure comprises the following steps:
step one: preparation of Al 2 O 3 YAG, ce/YAG composite fluorescent ceramic.
S1-1, proportioning: according to Al 2 O 3 The stoichiometric ratio of each element in the YAG to Ce is respectively calculated by the weight of aluminum oxide, yttrium oxide and cerium oxide, al 2 O 3 The mass ratio was 10.0wt.%, and the Ce doping level was 0.2at.%. Alumina, yttria and ceria are respectively weighed according to the stoichiometric ratio of each element in YAG.
S1-2, ball milling: the method comprises the steps of respectively mixing two groups of raw material powder by taking alumina balls as a medium and alcohol as a solvent, wherein the ball milling time is 24 hours, and the rotating speed is 170r/min.
S1-3, sieving: and (3) drying and sieving the mixed powder, wherein the drying temperature is 55 ℃, the drying time is 25 hours, and the sieving number is 200 meshes.
S1-4, tabletting: firstly, carrying out compression molding on YAG powder by adopting a dry press, wherein the pressure is 3MPa, and the pressure maintaining time is 5min; subsequently Al is added 2 O 3 YAG, ce powder is poured into a grinding tool to be pressed for the second time, the pressure is 10Mpa, and the pressure maintaining time is 5min.
S1-5, cold isostatic pressing: further compacting the pressed biscuit by adopting a cold extruder, wherein the pressure is 200Mpa, and the pressure maintaining time is 15min.
S1-6, vacuum sintering: and (3) putting the compacted biscuit into a vacuum sintering furnace, sintering the biscuit at 1770 ℃ for 12 hours.
S1-7, cutting: cutting the sintered ceramic by using a cutting machine, wherein the side length of the cut ceramic square sheet is 1.0 x 1.0mm, and the thickness is 0.6mm, wherein Al 2 O 3 YAG, ce complex phase ceramic 1 layer thickness is 0.3mm, YAG transparent ceramic 2 layer thickness is 0.3mm.
Step two: and preparing the fluorescent ceramic device with the composite structure.
S2-1, tabletting: adopting a dry press to perform Al 2 O 3 The powder is pressed and molded, the pressure is 3Mpa, and the pressure maintaining time is 5min; and then, the obtained biscuit and the ceramic square sheet obtained in the step S1-7 are pressed and molded again, the pressure is 10Mpa, and the pressure maintaining time is 5min.
S2-2, cold isostatic pressing: compacting the pressed biscuit by adopting a cold extruder; the compaction pressure of the cold extruder is 200Mpa and the dwell time is 15min.
S2-3, sintering and annealing: placing the compacted biscuit into a muffle furnace for sintering; the sintering temperature is 1450 ℃, and the sintering time is 12 hours.
S2-4, washing, grinding and polishing: surface treatment is carried out by a milling machine and a polishing machine to obtain Al 2 O 3 -YAG:Ce/YAG/Al 2 O 3 The diameter of the fluorescent ceramic with the composite structure is 20.0mm, and the thickness is 0.6mm. Wherein Al is 2 O 3 The thickness of the ceramic 3 is 0.6mm, al 2 O 3 YAG, ce complex phase ceramic 1 layer thickness is 0.3mm, YAG transparent ceramic 2 layer thickness is 0.3mm.
As shown in FIG. 2, blue light passes through the film layer 4 and YAG transparent ceramic 2 to excite Al 2 O 3 YAG-Ce complex phase ceramic 1, wherein part of generated fluorescence is emitted from the surface, part of the fluorescence is emitted downwards and is reflected back to the front direction, and the other part of the fluorescence is emitted to the periphery and passes through Al 2 O 3 The scattering of the ceramic 3 is returned to the forward direction. Laser testing is carried out on the fluorescent ceramic device with the composite structure, and when the laser power density is from 1.0W/mm to 60W/mm 2 The luminescence of the ceramic does not appear to be saturated. The surface temperature of the fluorescent ceramic device with the composite structure is increased from 25 ℃ to 103 ℃, and the luminous efficiency is reduced from 181.5lm/W to 164.2lm/W.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A fluorescent ceramic with a composite structure is characterized by comprising Al arranged up and down 2 O 3 -YAG: ce composite ceramic (1) and YAG transparent ceramic (2), and bordured Al 2 O 3 Ceramic (3).
2. The method for preparing the fluorescent ceramic with the composite structure according to claim 1, comprising the following steps:
step one: preparation of Al 2 O 3 -YAG: ce/YAG composite fluorescent ceramic;
s1-1, proportioning: according to Al 2 O 3 The stoichiometric ratio of each element in Ce is respectively calculated by the weight of aluminum oxide, yttrium oxide and cerium oxide; respectively weighing aluminum oxide and yttrium oxide according to the stoichiometric ratio of each element in YAG;
s1-2, ball milling: mixing two groups of raw material powder respectively by taking alumina balls as a medium and alcohol as a solvent;
s1-3, sieving: drying and sieving the mixed powder;
s1-4, tabletting: adopting a dry press to press and mold YAG powder; subsequently Al is added 2 O 3 Pouring YAG Ce powder into a grinding tool for secondary pressing;
s1-5, cold isostatic pressing: compacting the pressed biscuit by adopting a cold extruder;
s1-6, vacuum sintering: placing the compacted biscuit into a vacuum sintering furnace, and sintering the biscuit;
s1-7, cutting: cutting the sintered ceramic by using a cutting machine;
step two: preparing a fluorescent ceramic device with a composite structure;
s2-1, tabletting: adopting a dry press to perform Al 2 O 3 Compacting and forming the powder; then, the obtained biscuit and the ceramic square sheet obtained in the step S1-7 are pressed and formed again;
s2-2, cold isostatic pressing: compacting the pressed biscuit by adopting a cold extruder;
s2-3, sintering and annealing: placing the compacted biscuit into a muffle furnace for sintering;
s2-4, washing, grinding and polishing: surface treatment is carried out by a milling machine and a polishing machine to obtain Al 2 O 3 -YAG:Ce/YAG/Al 2 O 3 Fluorescent ceramics with composite structure.
3. The method according to claim 2, wherein in S1-1, al 2 O 3 YAG-Al in Ce 2 O 3 The mass ratio is 10.0-40.0 wt.%, and the Ce doping degree is 0.2-1.0 at.%.
4. The preparation method according to claim 2, wherein in S1-2, the ball milling time is 24 hours, and the rotating speed is 140-170 r/min.
5. The preparation method according to claim 2, wherein in S1-3, the drying temperature is 55 ℃ and the drying time is 15-20 h; the number of the screening meshes is 100-200 meshes.
6. The preparation method according to claim 2, wherein in S1-4, the dry press presses YAG powder for the first time at a pressure of 3MPa for a dwell time of 1-5 min; the secondary pressing pressure is 10Mpa, and the pressure maintaining time is 1-5 min; in S1-5, the compaction pressure of the cold extruder is 200Mpa, and the dwell time is 10-15 min.
7. The preparation method according to claim 2, wherein in S1-6, the sintering temperature is 1740-1770 ℃ and the heat preservation time is 12h; in S2-3, the sintering temperature is 1350-1450 ℃ and the sintering time is 12h.
8. The method according to claim 2, wherein Al is obtained by the process of steps S1-7 2 O 3 YAG (yttrium aluminum garnet) -Ce composite ceramic (1) layer with thickness of 0.1-0.3 mm and YAG transparent ceramicThe thickness of the ceramic (2) layer is 0.1-0.3 mm, the side length of the cut ceramic square sheet is 1.0 x 1.0mm, and the thickness is 0.2-0.6 mm.
9. The method according to claim 2, wherein in S2-1, the dry press is used for the production of Al 2 O 3 The powder pressing pressure is 3Mpa, and the pressure maintaining time is 1-5 min; the pressure of the secondary compression molding is 10Mpa, and the pressure maintaining time is 1-5 min; in S2-2, the compaction pressure of the cold extruder is 200Mpa, and the dwell time is 10-15 min.
10. The method according to claim 2, wherein Al is added in step S2-4 2 O 3 The thickness of the ceramic (3) is 0.2-0.6 mm, al 2 O 3 The thickness of the Ce composite ceramic (1) layer is 0.1-0.3 mm, and the thickness of the YAG transparent ceramic (2) layer is 0.1-0.3 mm; the diameter of the fluorescent ceramic with the composite structure is 16.0-20.0 mm, and the thickness is 0.2-0.6 mm.
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