CN111285682A - Full-spectrum complex phase fluorescent ceramic for laser illumination and display and preparation method thereof - Google Patents
Full-spectrum complex phase fluorescent ceramic for laser illumination and display and preparation method thereof Download PDFInfo
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- 238000001228 spectrum Methods 0.000 title claims abstract description 17
- 238000005286 illumination Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims description 9
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 36
- 238000005245 sintering Methods 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 235000015895 biscuits Nutrition 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 9
- 238000009694 cold isostatic pressing Methods 0.000 claims description 7
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 229910052706 scandium Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
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- 239000002223 garnet Substances 0.000 claims description 2
- 238000001513 hot isostatic pressing Methods 0.000 claims description 2
- 238000009768 microwave sintering Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 238000003980 solgel method Methods 0.000 claims description 2
- 238000002490 spark plasma sintering Methods 0.000 claims description 2
- 238000010345 tape casting Methods 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims 2
- 238000005266 casting Methods 0.000 claims 1
- 238000007731 hot pressing Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000009877 rendering Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 24
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a full-spectrum complex phase fluorescent ceramic for laser illumination and laser display, which comprises a first phase and a chemical composition (A)2‑xCexMg)MyAl5‑y‑zDzO12(ii) a And a second phase of chemical composition (Y, Lu)3‑tRetAl5O12. The invention has the beneficial effects that: the LED light source has a completely compact microstructure, excellent thermal conductivity and mechanical property, effectively improves light extraction efficiency, and can greatly improve final light efficiency, so that the problems of insufficient absorption of incident blue light, too low color rendering index and the like are solved, and a light source which emits light more uniformly and has higher color quality is obtained.
Description
Technical Field
The invention relates to the field of fluorescent materials for laser illumination, in particular to a full-spectrum complex phase fluorescent ceramic for laser illumination and laser display and a preparation method thereof.
Background
The light source equipment for exciting the fluorescent ceramic by the laser light source has the advantages of high brightness, high light efficiency, long irradiation distance, long service life, small size and the like, can be widely applied to the fields of aviation, aerospace, navigation illumination, projection display and the like, and is expected to be widely applied to indoor illumination and various portable illuminations in the future.
The fluorescent ceramic is excited by the light emitted by the laser source, and the emission of white light and multicolor light is realized by wavelength conversion, however, the current light source equipment for exciting the fluorescent ceramic by the laser source mainly has the following outstanding problems: wide-spectrum light emission from green light to red light is difficult to realize in fluorescent ceramics with the same component under the excitation of blue light; the fluorescent ceramic contains pores, second phase defects, inversion defects and the like, and phenomena such as scattering, absorption, luminescence center quenching and the like can be generated, so that the luminous efficiency is reduced.
The existing fluorescent ceramics mainly realize spectrum broadening by single-phase multiple-luminescent-ion doping (J.Eur.Ceram. Soc.373403-3409 (2017)) or multiple-phase multilayer structure design (Opt.express 23 (14)) 18243-55(2015)), but the modes are difficult to avoid reduction of luminous efficiency and cannot realize wide-spectrum emission of blue light excitation.
Disclosure of Invention
The invention provides a full-spectrum complex phase fluorescent ceramic material which can be excited by a blue light emitting semiconductor laser diode, consists of two different phase substances and can be used for manufacturing high color rendering white light laser illumination and projection display equipment.
The technical scheme of the invention is as follows: a fluorescent full spectrum multiphase fluorescent ceramic material has a chemical formula of (A)2-xCexMg)MyAl5-y-zDzO12/(Y,Lu)3-tRetAl5O12Wherein A is at least one of La, Gd, Tb, Yb, Lu, Y, Sc and Bi, M is at least one of Mg, Ca, Sr, Sc and B, D is at least one of Ga, In, Zr, Si, Ti and Ge, Re is at least one of Ce, Pr, Eu, Tb, Dy, Cr and Mn, x is more than or equal to 0.0005 and less than or equal to 1.5, Y is more than or equal to 0 and less than or equal to 1.5, z is Y +1, and t is more than or equal to 0.001 and less than or equal to 1; preferably, 0.005. ltoreq. x.ltoreq.0.1.
At least one of the two phases of the complex phase fluorescent ceramic material is of a garnet structure, belongs to a cubic crystal system, and has a space group Ia3 d.
The excitation wavelength of the complex phase fluorescent ceramic material is 400-490nm, preferably, the excitation wavelength can be effectively excited by blue light at 430-480nm, and the emission wavelength range is 510-780nm under the excitation of the blue light.
The spectrum of the fluorescent ceramic material can be adjusted by adjusting the matrix components and the types and concentrations of rare earth elements, so that low color temperature and high color development are achieved.
The invention also provides a method for preparing the complex phase fluorescent ceramic material, which comprises the following steps:
(1) according to (A)2-xCexMg)MyAl5-y-zDzO12/(Y,Lu)3-tRetAl5O12Respectively weighing an oxide or a corresponding salt of A, an oxide or a corresponding salt of Ce, an oxide or a corresponding salt of Mg, an oxide or a corresponding salt of Al, and an oxide or a corresponding salt of B as the component 1; yttrium oxide or its salt, lutetium oxide or its salt, Re oxide or its salt as component 1, mixing or dissolving the two components, and dryingThen two nano or submicron powder are obtained;
(2) calcining the powder, removing organic matters and residual media or solvents in the powder, mechanically mixing the two kinds of powder according to a certain weight percentage, and forming the mixed powder to obtain a ceramic biscuit;
(3) pre-sintering the ceramic biscuit at the temperature of 600-1300 ℃ for 2 hours in a heat preservation way;
(4) and (3) sintering and annealing the pre-sintered sample at high temperature to obtain the fully compact complex phase fluorescent ceramic (5), and grinding and polishing the complex phase fluorescent ceramic.
In the step (1), the method for obtaining the mixed or powder is not limited, and includes a ball milling method, a sol-gel method or a coprecipitation method;
in the step (1), the powder drying method is not limited, and comprises microwave drying, water bath rotary heating drying, direct drying and the like;
in the step (2), the components with the weight percentage of 1 are preferably selected: component 2 is 1/6-1/2;
in the step (2), the powder mixing mode is not limited, and comprises manual mixing of a mortar, mixing of a double-roller mixer, mixing of a three-dimensional mixer, mixing of a V-shaped mixer and mixing of a double-cone mixer;
in the step (2), the powder forming mode is not limited, and comprises dry pressing, tape casting, gel injection molding, 3D printing, cold isostatic pressing and the like;
in the step (3), the pre-sintering temperature is preferably 800-1100 ℃;
in the step (4), the high-temperature sintering mode is not limited, and comprises microwave sintering, vacuum sintering, oxygen atmosphere sintering and H2Or CO atmosphere sintering, hot isostatic pressing sintering, spark plasma sintering, hot press sintering, and the like. Preferably, the sintering process is divided into two stages: firstly heating to 1000-1400 ℃, preserving heat for 0.5-10 h, then heating to 1600-1900 ℃, preserving heat for 2-50 h, wherein the pressure is 1 x 10 according to different sintering modes-3Pa-300 Mpa;
in the step (4), the annealing method is not limited, and comprises the steps of performing in air, reducing atmosphere and oxygen atmosphere, preferably annealing at 900-1400 ℃, preferably keeping the temperature for 2-50 h, and then cooling to room temperature to obtain the complex phase fluorescent ceramic.
Compared with the prior art, the invention has the beneficial effects that: the full-inorganic full-spectrum fluorescent ceramic material is obtained by doping composite two-phase matrix components and multiple rare earth luminescent ions, compared with single-phase fluorescent ceramic, the complex-phase fluorescent ceramic material has a completely compact microstructure, excellent thermal conductivity and mechanical property, can be directly used for laser illumination and laser projection display equipment after laser or mechanical cutting, can effectively improve light extraction efficiency due to the composition of two phases, and can greatly improve final light efficiency, so that the problems of insufficient absorption of incident blue light, too low color rendering index and the like are solved, and a light source which emits light more uniformly and has higher color quality is obtained.
Drawings
Fig. 1 is an excitation spectrum of the complex phase fluorescent ceramic sheet in example 1 of the present invention.
Fig. 2 is a graph showing an emission spectrum of the complex phase fluorescent ceramic sheet according to example 1 of the present invention.
Fig. 3 is an excitation spectrum of the complex phase fluorescent ceramic sheet in example 2 of the present invention.
Fig. 4 is a spectrum of the emission light of the complex phase fluorescent ceramic sheet in example 2 of the present invention.
Fig. 5 is a scanning electron microscope photograph of the complex phase fluorescent ceramic sheet according to example 2 of the present invention.
Fig. 6 is an excitation and emission spectrum of the complex phase fluorescent ceramic sheet in example 3 of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to specific embodiments and drawings.
Example 1:
fluorescent ceramic plate (Lu)1.98Ce0.02Mg)MgAl3SiO12/Y1.475Lu1.475Ce0.05Al5O12The preparation method comprises the following steps:
(1) the following mixture ratio is obtained by stoichiometric calculation:
adding alumina balls into a grinding tank, and grinding and mixing by taking absolute ethyl alcohol as a grinding medium until the average particle size of the powder is less than 1 mu m;
(2) drying and sieving the obtained slurry, and keeping the sieved powder at 1000 ℃ in the air for 2 hours to remove organic matters in the powder; sieving the obtained powder, keeping under 4MPa for 2min, dry-pressing, and pressing into biscuit with cold isostatic pressing equipment under 200MPa for 5 min;
(3) sintering the obtained ceramic biscuit in a vacuum furnace, wherein the heating rate is 1 ℃/min, the temperature is kept at 900 ℃ for 3h, the temperature is kept at 1780 ℃ for 12h, the solid-phase reaction is completed, and the densification is achieved by removing air holes;
(4) the sample after vacuum sintering is put in the air, the temperature is kept at 1100 ℃ for 6h for annealing, and the obtained fluorescent ceramic is polished to obtain (Lu)1.98Ce0.02Mg)MgAl3SiO12/Y1.475Lu1.475Ce0.05Al5O12The thickness of the fluorescent ceramic plate is 1 mm.
The excitation emission spectrum of the fluorescent ceramic sheet prepared above is shown in fig. 1 and 2.
Example 2:
fluorescent ceramic plate (Lu)1.95Ce0.05Mg)Mg0.5Al3Si1.5O12/Y1.5Lu1.5Cr0.05Al4.95O12The preparation method comprises the following steps:
(1) the following mixture ratio is obtained by stoichiometric calculation:
adding alumina balls into a grinding tank, and grinding and mixing by taking absolute ethyl alcohol as a grinding medium until the average particle size of the powder is less than 1 mu m;
(2) drying and sieving the obtained slurry, and keeping the sieved powder at 850 ℃ in the air for 2h to remove organic matters in the powder; sieving the obtained powder, applying 2MPa pressure for 2min by using equiaxial one-way, dry-pressing for molding, and pressing into biscuit in cold isostatic pressing equipment with pressure of 250MPa and pressure maintaining time of 5 min;
(3) sintering the obtained ceramic biscuit in a vacuum furnace, wherein the heating rate is 5 ℃/min, the temperature is kept at 1000 ℃ for 6h, the temperature is kept at 1650 ℃ for 10h, the solid-phase reaction is completed, and the densification is achieved by removing air holes;
(4) the sample after vacuum sintering is put in the air, the temperature is kept at 1400 ℃ for 6h for annealing, and the obtained fluorescent ceramic is polished to obtain (Lu)1.95Ce0.05Mg)Mg0.5Al3Si1.5O12/Y1.5Lu1.5Cr0.05Al4.95O12The thickness of the fluorescent ceramic sheet is 0.5 mm. .
The excitation emission spectra of the fluorescent ceramic sheet prepared above are shown in fig. 3 and 4, and also in fig. 5.
Example 3:
fluorescent ceramic plate (Y)1.95Ce0.05Mg)CaAl3SiO12/Y1.475Lu1.475Pr0.05Cr0.05Al4.95O12The preparation method comprises the following steps:
(1) the following mixture ratio is obtained by stoichiometric calculation:
adding alumina balls into a grinding tank, and grinding and mixing by taking absolute ethyl alcohol as a grinding medium until the average particle size of the powder is less than 1 mu m;
(2) drying and sieving the obtained slurry, and keeping the sieved powder at 900 ℃ in the air for 4 hours to remove organic matters in the powder; sieving the obtained powder, keeping the powder under 3MPa for 1min by using equiaxial one-way pressure, performing dry pressing, and pressing the powder into a biscuit in cold isostatic pressing equipment under the pressure of 250MPa for 1 min;
(3) sintering the obtained ceramic biscuit in a vacuum furnace, wherein the heating rate is 1 ℃/min, the temperature is kept at 1000 ℃ for 2h, the temperature is kept at 1750 ℃ for 8h, the solid-phase reaction is completed, and the densification is achieved by removing air holes;
(4) the sample after vacuum sintering is put in the air, the temperature is kept at 1300 ℃ for 20h for annealing, and the obtained fluorescent ceramic is polished to obtain (Y)1.95Ce0.05Mg)CaAl3SiO12/Y1.475Lu1.475Pr0.05Cr0.05Al4.95O12The thickness of the fluorescent ceramic plate is 1 mm.
The excitation emission spectrum of the prepared fluorescent ceramic sheet is shown in fig. 6, which shows that the ceramic material can realize the simultaneous and efficient emergence of three characteristic emission peaks.
Example 4:
fluorescent ceramic plate (Gd)1.95Ce0.05Mg)CaScAl2SiO12/Y1.475Lu1.475Ce0.05Al5O12The preparation method comprises the following steps:
(1) the following mixture ratio is obtained by stoichiometric calculation:
adding alumina balls into a grinding tank, and grinding and mixing by taking absolute ethyl alcohol as a grinding medium until the average particle size of the powder is less than 1 mu m;
(2) drying and sieving the obtained slurry, and keeping the sieved powder at 1100 ℃ in the air for 2 hours to remove organic matters in the powder; sieving the obtained powder, keeping the powder under 3MPa for 0.5min by using equiaxial one-way application, performing dry pressing, and pressing the powder into a biscuit in cold isostatic pressing equipment under the pressure of 200MPa for 3 min;
(3) sintering the obtained ceramic biscuit in a vacuum furnace, wherein the heating rate is 5 ℃/min, the temperature is kept at 1200 ℃ for 1h, the temperature is kept at 1800 ℃ for 15h, the solid-phase reaction is completed, and the densification is achieved by removing air holes;
(4) the sample after vacuum sintering is put in air and annealed at 1450 ℃ for 10h to obtain the fluorescent ceramic which is polishedLight treatment to obtain (Gd)1.95Ce0.05Mg)CaScAl2SiO12/Y1.475Lu1.475Ce0.05Al5O12The thickness of the fluorescent ceramic plate is 1 mm.
The excitation emission spectrum of the fluorescent ceramic sheet prepared above is similar to that shown in fig. 1.
Example 5:
fluorescent ceramic plate (Gd)1.95Ce0.05Mg)SrAl3SiO12/Y1.475Lu1.475Ce0.05Al5O12The preparation method comprises the following steps:
(1) the following mixture ratio is obtained by stoichiometric calculation:
adding alumina balls into a grinding tank, and grinding and mixing by taking absolute ethyl alcohol as a grinding medium until the average particle size of the powder is less than 1 mu m;
(2) drying and sieving the obtained slurry, and keeping the sieved powder at 1000 ℃ in the air for 2 hours to remove organic matters in the powder; sieving the obtained powder, keeping under 6MPa for 2min, dry-pressing, and pressing into biscuit with cold isostatic pressing equipment under 250MPa for 10 min;
(3) sintering the obtained ceramic biscuit in a vacuum furnace, wherein the heating rate is 3 ℃/min, the temperature is kept at 1000 ℃ for 3h, the temperature is kept at 1700 ℃ for 12h, the solid-phase reaction is completed, and the densification is achieved by removing air holes;
(4) the sample after vacuum sintering is put in air and is annealed at 1400 ℃ for 12h, and the obtained fluorescent ceramic is polished to obtain (Gd)1.95Ce0.05Mg)SrAl3SiO12/Y1.475Lu1.475Ce0.05Al5O12The thickness of the fluorescent ceramic plate is 2 mm.
The excitation emission spectrum of the fluorescent ceramic sheet prepared above is similar to that shown in fig. 1.
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 (10)
1. The full-spectrum complex phase fluorescent ceramic for laser illumination and display is characterized by comprising,
a first phase of chemical composition (A)2-xCexMg)MyAl5-y-zDzO12；
Wherein A is one or more of La, Gd, Tb, Yb, Lu, Y, Sc and Bi, and M is one or more of Mg, Ca, Sr, Sc and B; d is one or more of Ga, In, Zr, Si, Ti and Ge;
wherein x is more than or equal to 0.0005 and less than or equal to 1.5, y is more than or equal to 0 and less than or equal to 1.5, z = y +1, further, x is more than or equal to 0.005 and less than or equal to 0.1, y is more than or equal to 0 and less than or equal to 1.5, and z = y + 1; and the number of the first and second groups,
the second phase has a chemical composition of (Y, Lu)3-tRetAl5O12；
Wherein Re is one or more of Ce, Pr, Eu, Tb, Dy, Cr and Mn;
wherein t is more than or equal to 0.001 and less than or equal to 1;
further, at least one of the first phase and the second phase has a garnet structure and belongs to a cubic system, space group Ia3 d;
further, a fully dense structure is formed between the first phase and the second phase, with no pores and other phases between the two.
2. The full spectrum complex phase fluorescent ceramic for laser illumination and display as claimed in claim 1, wherein the grain size of the first phase and the second phase are both in the range of 1-20 μm.
3. The preparation method of the full-spectrum complex phase fluorescent ceramic for laser illumination and display, which is used for preparing the full-spectrum complex phase fluorescent ceramic of claim 1 or 2, and is characterized in that: comprises the following steps of (a) carrying out,
step S1, preparing a powder of the first phase and a powder of the second phase, respectively;
a first phase of chemical composition (A)2-xCexMg)MyAl5-y-zDzO12；
Wherein A is one or more of La, Gd, Tb, Yb, Lu, Y, Sc and Bi, and M is one or more of Mg, Ca, Sr, Sc and B; d is one or more of Ga, In, Zr, Si, Ti and Ge;
wherein x is more than or equal to 0.0005 and less than or equal to 1.5, y is more than or equal to 0 and less than or equal to 1.5, z = y +1, further, x is more than or equal to 0.005 and less than or equal to 0.1, y is more than or equal to 0 and less than or equal to 1.5, and z = y + 1; and the number of the first and second groups,
the second phase has a chemical composition of (Y, Lu)3-tRetAl5O12；
Wherein Re is one or more of Ce, Pr, Eu, Tb, Dy, Cr and Mn;
wherein t is more than or equal to 0.001 and less than or equal to 1;
step S2, mixing the powder of the first phase and the powder of the second phase, and preparing a biscuit through a molding process;
step S3, pre-burning the biscuit in air at low temperature;
step S4, sintering at high temperature;
step S5, annealing; and the number of the first and second groups,
and step S6, grinding and polishing.
4. The method of claim 3, wherein the mixing step S1 is ball milling, sol-gel process or co-precipitation process.
5. The method for preparing the full spectrum complex phase fluorescent ceramic for laser illumination and display as claimed in claim 3, wherein the calcination at different temperatures in step S1 is 600-1000 deg.C, 800-1300 deg.C respectively.
6. The method of claim 3, wherein the mixing in step S2 is manual bowl mixing, three-dimensional blender mixing, V-blender mixing or double cone blender mixing.
7. The method of claim 3, wherein the step S2 is performed by dry pressing, tape casting, gel casting, 3D printing or cold isostatic pressing.
8. The method of claim 3, wherein the sintering step S4 is microwave sintering, vacuum sintering, oxygen atmosphere sintering, H-sintering2Or CO atmosphere sintering, hot isostatic pressing sintering, spark plasma sintering or hot pressing sintering.
9. The method of claim 3, wherein the annealing step S5 is performed in air, reducing atmosphere or oxygen atmosphere.
10. The method as claimed in claim 3, wherein the annealing in step S4 is performed at a temperature not exceeding 1100 ℃ and 1500 ℃ for a time not exceeding 60 hours to eliminate the internal stress of the ceramic.
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