CN107298582B - Ceramic material and preparation method thereof and fluorescent ceramic device - Google Patents
Ceramic material and preparation method thereof and fluorescent ceramic device Download PDFInfo
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- CN107298582B CN107298582B CN201710523795.8A CN201710523795A CN107298582B CN 107298582 B CN107298582 B CN 107298582B CN 201710523795 A CN201710523795 A CN 201710523795A CN 107298582 B CN107298582 B CN 107298582B
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 105
- 239000000919 ceramic Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000000843 powder Substances 0.000 claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 25
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 25
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 25
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 7
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052765 Lutetium Inorganic materials 0.000 claims description 6
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 230000005284 excitation Effects 0.000 abstract description 20
- 230000007423 decrease Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 11
- 150000002500 ions Chemical class 0.000 description 11
- 238000000498 ball milling Methods 0.000 description 10
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 10
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 7
- 238000001354 calcination Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000007873 sieving Methods 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000001748 luminescence spectrum Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000005562 fading Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 1
- 238000000875 high-speed ball milling Methods 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000003826 uniaxial pressing Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention provides a ceramic material consisting of Y2O3、Al2O3、CeO2And M oxide; and M is selected from one or more of Si, Ge, Ga, Sc and V. The ceramic material provided by the invention can generate green light with the peak wavelength less than or equal to 525nm and the half width of the luminous peak less than or equal to 70nm under the excitation of blue laser, the transparency of the ceramic material can be adjusted through the porosity, and the ceramic material has good thermal conductivity and thermal stability, so that the ceramic material can be prepared into a fluorescent ceramic device, can replace fluorescent powder to be used for a projection system, effectively avoids the thermal decline of the luminous brightness when the fluorescent powder is adopted, enables the projection system to have good color performance, ultra-long service life and good stability, and improves the output brightness of the system to the maximum extent.
Description
Technical Field
The invention relates to the technical field of multifunctional materials, in particular to a ceramic material, a preparation method thereof and a fluorescent ceramic device.
Background
Most of the current micro-projection adopts an LED as an illumination light source. The LED has the advantages of small volume, long service life, quick response, energy conservation, environmental protection and the like, but in the application of micro projection, the problems that the luminous flux of the LED is not high, the luminous flux on unit optical expansion is lower than that of the traditional projection light source, the heat productivity is overlarge and the like still exist. In order to improve the luminous efficiency of the LED, a fluorescent powder technology can be adopted, and LEDs with other wavelengths are prepared by utilizing the advantage of high luminous efficiency of LEDs with certain wavelengths, so that the luminous efficiency of the waveband is improved. However, the spectrum range is too wide, the color purity is greatly reduced, and the light-emitting angle is increased after the LED excites the fluorescent powder, which brings pressure to the design of the subsequent optical system.
The manner in which the LED excites the phosphor does not meet the requirements of high brightness projection systems. In order to realize high-brightness projection output, LD laser with high energy density is used as a light source, and excitation of primary color phosphor to generate higher-brightness primary color light becomes a necessary choice. The high brightness characteristic of laser and the low interference generated by fluorescent powder are used to weaken the speckle of laser image. In the prior art, the primary color fluorescent powder and silica gel are mixed and coated on a color wheel, and a laser light source irradiates on the fluorescent powder color wheel to generate primary color light through excitation. Blue laser with high energy is generally used as a light source to excite green phosphor and red phosphor. Since the laser has a high energy density, the color wheel must rotate at a high speed to avoid phosphor aging and even burning due to excessive local temperature. However, even when the phosphor is rotated at a high speed, the phosphor is thermally quenched by the high-temperature irradiation, which results in a decrease in the light emission intensity of the phosphor. Finally, the light extraction efficiency is obviously reduced along with the prolonging of the service time, which is especially obvious on high-power illumination. The lifetime of the color wheel phosphor is usually only thousands of hours, which seriously affects the lifetime and color performance of the projector.
Therefore, a light emitting device replacing fluorescent powder for a high brightness projection system is urgently needed in the market at present, so that the projector has better color performance, ultra-long service life and good stability, and the output brightness of the system is improved.
Disclosure of Invention
In view of the above, the present invention provides a ceramic material, a method for preparing the same, and a fluorescent ceramic device, which has good color performance, life and stability when used in a projection system.
The invention provides a ceramic material consisting of Y2O3、Al2O3、CeO2And M oxide;
and M is selected from one or more of Si, Ge, Ga, Sc and V.
Preferably, the raw materials for preparing the ceramic material also comprise an oxide of R, wherein the R is selected from one or more of La, Pr, Sm, Tb, Dy and Lu;
the molar ratio of Y, Ce, R, Al and M in the ceramic material is (3-x-Y): x: y (5-z): z;
0.001≤x≤0.06；
0≤y≤0.06；
0.05≤z≤2。
the invention provides a preparation method of the ceramic material in the technical scheme, which comprises the following steps:
(1) will Y2O3、Al2O3、CeO2Mixing with the oxide of M to prepare a powder raw material;
(2) pressing and molding the powder raw material to obtain a green body;
(3) and sintering the green body to obtain the ceramic material.
Preferably, the pressure in the compression molding process in the step (2) is more than or equal to 200 MPa.
Preferably, the method for press forming in step (2) is cold isostatic pressing.
Preferably, the sintering temperature in the step (3) is 1400-1750 ℃.
Preferably, the sintering time in the step (3) is 5-20 hours.
Preferably, the sintering in the step (3) is sintering under vacuum condition;
vacuum degree of not less than 3 × 10-3Pa。
Preferably, the sintering in the step (3) is sintering in an oxygen atmosphere;
the pressure of oxygen is 0.01 to 0.1 MPa.
The invention provides a fluorescent ceramic device which comprises the ceramic material in the technical scheme.
Compared with the prior art, the invention adopts specific raw materials to prepare the ceramic material, and the ceramic material is prepared by Ce3+The active ion is the main active ion, the M ion is doped or the M ion and the R ion are simultaneously doped to adjust the luminous peak position of the ceramic material, so that the ceramic material can generate green light with the peak wavelength less than or equal to 525nm and the luminous peak half-width height less than or equal to 70nm under the excitation of blue laser, and meanwhile, the transparency of the ceramic material can be adjusted through the porosity, so that the ceramic material has good color performance. The ceramic material has good thermal conductivity and thermal stability, and can be prepared into fluorescent ceramic devices to replace fluorescent powderThe projection system effectively avoids the heat fading of the luminous brightness when the fluorescent powder is adopted, so that the projection system has good color performance, ultra-long service life and good stability, and the output brightness of the system is improved to the maximum extent.
Drawings
FIG. 1 shows a luminescence spectrum of a ceramic material prepared in example 1 of the present invention under excitation of blue light of 450 nm.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The invention provides a ceramic material consisting of Y2O3、Al2O3、CeO2And M oxide;
and M is selected from one or more of Si, Ge, Ga, Sc and V.
In the invention, the preparation raw material of the ceramic material preferably further comprises an oxide of R, wherein R is selected from one or more of La, Pr, Sm, Tb, Dy and Lu.
The present invention provides a ceramic material, preferably consisting of Y2O3、Al2O3、CeO2The oxide of R and the oxide of M;
r is selected from one or more of La, Pr, Sm, Tb, Dy and Lu;
and M is selected from one or more of Si, Ge, Ga, Sc and V.
In the present invention, when R is selected from several of La, Pr, Sm, Tb, Dy and Lu, the oxide of R may be an oxide formed by a plurality of elements or a mixture of oxides formed by the respective elements. In the present invention, when M is selected from several of Si, Ge, Ga, Sc, and V, the oxide of M may be an oxide formed by a plurality of elements or a mixture of oxides formed by the respective elements.
In the present inventionThe molar ratio of Y, Ce, R, Al and M in the ceramic material is preferably (3-x-Y): x: y (5-z): z; x is more than or equal to 0.001 and less than or equal to 0.06; y is more than or equal to 0 and less than or equal to 0.06, and z is more than or equal to 0.05 and less than or equal to 2; when y is 0, the raw materials for preparing the ceramic material do not contain the oxide of R, and the preferable range is 0 < y ≦ 0.06. In the present invention, the chemical composition of the ceramic material may be (Y)3-x-yCexRy)(Al5-zMz)O12And (4) showing.
The invention provides a preparation method of the ceramic material in the technical scheme, which comprises the following steps:
(1) will Y2O3、Al2O3、CeO2Mixing with the oxide of M to prepare a powder raw material; the powder raw material preferably further contains an oxide of R;
(2) pressing and molding the powder raw material to obtain a green body;
(3) and sintering the green body to obtain the ceramic material.
In the present invention, the oxide of R and the oxide of M are the same as those described in the above technical solutions, and are not described herein again. The invention is directed to said Y2O3、Al2O3、CeO2The sources of the oxide of R and the oxide of M are not particularly limited and commercially available, and the purity of each oxide is preferably not less than 99.9%. In the present invention, said Y is2O3、Al2O3、CeO2The use amount ratio of the oxide of R and the oxide of M can ensure that the molar ratio of Y, Ce, R, Al and M in the prepared ceramic material meets the molar ratio in the technical scheme.
The invention will Y2O3、Al2O3、CeO2The method for preparing the powder raw material from the mixture of the oxide of R and the oxide of M is not particularly limited, and the powder raw material can be prepared by a solid phase ball milling method or a wet chemical method well known to those skilled in the art.
In the invention, the raw materials for preparing the powder by the solid phase ball milling method are preferably as follows:
will Y2O3、Al2O3、CeO2Carrying out ball milling on the oxide of R and the oxide of M in a ball milling medium, a sintering aid and a dispersing agent to obtain a mixture;
drying, grinding and sieving the obtained mixture, and calcining to obtain a calcined product;
and sieving the obtained calcined product again to obtain a powder raw material.
In the present invention, the ball milling medium is preferably absolute ethanol. In the present invention, the sintering aid is preferably tetraethyl orthosilicate. In the present invention, the dispersant is preferably polyethylene glycol, more preferably polyethylene glycol 400.
In the present invention, the grinding balls in the ball milling process are preferably alumina balls, and more preferably high-purity alumina balls. In the present invention, the apparatus for ball milling is preferably a planetary ball mill.
The invention obtains submicron grade high purity powder by drying, grinding and sieving the mixture after ball milling. The invention calcines the sieved powder to remove residual organic matters. In the invention, the calcining temperature is preferably 700-800 ℃, and more preferably 750 ℃; the calcination time is preferably 0.5 to 2 hours, and more preferably 1 hour. The invention can obtain submicron grade high-purity superfine powder raw material by sieving the obtained calcined product again.
In the invention, the wet chemical preparation powder raw material is preferably prepared by a urea precipitation method, and specifically comprises the following steps:
will Y2O3、Al2O3、CeO2Dissolving the oxide of R and the oxide of M in nitric acid to obtain a nitrate solution;
mixing and diluting a nitrate solution, a urea solution and an ammonium sulfate solution to obtain a mixed solution;
reacting the mixed solution at constant temperature, standing, and collecting precipitate;
washing, drying and grinding the precipitate to obtain precursor powder;
and calcining the precursor powder at high temperature to obtain a powder raw material.
In the invention, the content of urea in the mixed solution is preferably 50-100 times of the concentration of nitrate; the molar amount of ammonium sulfate is preferably equivalent to the molar amount of nitrate. In the present invention, the concentration of the nitrate in the mixed solution is preferably 0.001 to 0.03mol/L, more preferably 0.005 to 0.025mol/L, and most preferably 0.01 to 0.02 mol/L.
In the invention, the constant temperature condition is preferably 80-99 ℃, more preferably 85-95 ℃, and most preferably 90 ℃. In the present invention, the reaction time is preferably 2 to 5 hours. In the present invention, it is preferable to collect the precipitate by filtration.
In the invention, the high-temperature calcination temperature is preferably 800-1100 ℃, and more preferably 900-1000 ℃. In the invention, the high-temperature calcination time is preferably 2-5 hours.
In the invention, the purity of the powder raw material is preferably not lower than 99.9%; the particle size of the powder raw material is preferably 100 nm-1000 nm, more preferably 200-800 nm, and most preferably 300-600 nm.
The invention presses and shapes the powder raw material, preferentially carries on the single-shaft pressing and shapes the powder raw material, then carries on the cold isostatic pressing, gets the green compact with certain intensity. In the present invention, the pressure of the cold isostatic pressing is preferably 200MPa or more.
In the invention, the sintering temperature is preferably 1400-1750 ℃, more preferably 1450-1700 ℃, and most preferably 1500-1600 ℃, in the invention, the sintering time is preferably 5-20 hours, more preferably 10-15 hours, in the invention, the sintering is preferably carried out under a vacuum condition, and the vacuum degree is preferably not lower than 3 × 10-3Pa. In the present invention, the sintering may be performed in an oxygen atmosphere, and the oxygen pressure is preferably 0.01 to 0.1MPa, more preferably 0.03 to 0.07MPa, and most preferably 0.05 MPa.
In the present invention, the selection of doping elements (M element or M and R element doped simultaneously) and their doping amounts has a great influence on the sintering process, for example, when the doping amount of La is large, the sintering temperature can be properly reduced or the heat preservation time can be shortened, and when the doping amount of Sc is large, the sintering temperature needs to be properly increased or the heat preservation time needs to be prolonged.
The invention preferably carries out molding, cold isostatic pressing and oxygen atmosphere sintering on the powder raw material to obtain the ceramic material with fine crystal grains, uniform size and extremely low porosity, and the ceramic material is fluorescent ceramic.
The invention provides a fluorescent ceramic device which comprises the ceramic material in the technical scheme. The fluorescent ceramic device is prepared from the ceramic material according to the technical scheme, the preparation method is not particularly limited, and a person skilled in the art can select a proper method according to actual conditions to prepare the ceramic material into the ceramic device. In the invention, the ceramic material obtained by the technical scheme can be cut into pieces according to the size requirement and then subjected to surface planarization to obtain the required fluorescent ceramic device.
The ceramic material prepared by the invention has high crystallinity, uniform grain size and extremely low porosity; ce3+Mainly active ion, has high absorption efficiency to blue light, and is doped with La3+、Pr3+、Sm3+、Tb3+、Dy3+、Lu3+Or Si4+、Ge4+、Ga3+、Sc3+、V3+One or more of them to change Ce3+Crystal field of the ion, so that Ce is3+The fluorescent ceramic material generates green light with peak wavelength less than or equal to 525nm under the excitation of blue light LD, and the full width at half maximum of the luminescent peak is less than or equal to 70 nm.
The ceramic material and the fluorescent ceramic device provided by the invention are used for a projection system, and the fluorescent ceramic device is used for replacing a fluorescent powder color wheel in a traditional micro-projection system, so that the luminous performance of silica gel packaged fluorescent powder can be effectively prevented from being obviously attenuated, the luminous brightness stability is improved, and the service life is greatly prolonged.
For further understanding of the present invention, the following examples are given for the purpose of illustrating the ceramic material provided by the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
The required high-purity Y is weighed according to the mol ratio of 2.998:4.95:0.002:0.001:0.12O3、Al2O3、CeO2、La2O3And SiO2The purity of the product is not less than 99.9 percent, and then absolute ethyl alcohol is used as a ball milling medium, high-purity alumina balls are used as grinding balls, tetraethoxysilane is used as a sintering aid, polyethylene glycol 400 is used as a dispersing agent, and the product is subjected to high-speed ball milling in a planetary ball mill. Drying, grinding and sieving after ball milling to obtain submicron grade high purity powder, calcining the powder at 750 ℃ for 1 hour to remove residual organic matters, and sieving again after calcining to obtain submicron grade high purity superfine powder raw material.
Carrying out uniaxial pressing on the obtained superfine powder raw material, and then carrying out cold isostatic pressing at 250MPa to obtain a green compact sheet with certain strength;
sintering the obtained green sheet in an atmosphere furnace at 1600 deg.C for 10 hr under oxygen pressure of 0.05MPa to obtain (Y)2.998Ce0.001La0.001)(Al4.95Si0.05)O12A ceramic material.
The transmittance of the ceramic material prepared in example 1 of the present invention was measured by an ultraviolet-visible spectrophotometer, and the result of the measurement shows that the ceramic material obtained in example 1 of the present invention has a transmittance of 78% at a wavelength of 500nm or more, and is a transparent ceramic.
The heat conductivity of the ceramic material prepared in the embodiment 1 of the method is tested by using a heat flow sensor, and the test result shows that the ceramic material prepared in the embodiment 1 of the invention has the heat conductivity of 11.3W/m.K and has good heat conductivity.
The luminescence intensities of the ceramic material prepared in the embodiment 1 of the present invention at 25 ℃, 50 ℃, 100 ℃, 150 ℃ and 200 ℃ were respectively tested by a fluorescence spectrometer (in cooperation with a cryostat), and the luminescence intensity at 25 ℃ was recorded as 1; as a result of the test, the ceramic material obtained in example 1 of the present invention has luminescence intensities of 0.992, 0.963, 0.941, and 0.913 at 50 deg.C, 100 deg.C, 150 deg.C, and 200 deg.C, respectively, and has good thermal stability.
The fluorescence spectrometer is used to test the luminescence spectrum of the ceramic material prepared in the embodiment 1 of the present invention under the excitation of blue light of 450nm, the test result is shown in fig. 1, and fig. 1 is the luminescence spectrum of the ceramic material prepared in the embodiment 1 of the present invention under the excitation of blue light of 450 nm. As can be seen from FIG. 1, the ceramic material prepared in example 1 of the present invention can generate green light under the excitation of blue light, the luminescent peak position of the green light is 525nm, the half-width height of the luminescent peak is less than or equal to 70nm, and the fluorescence conversion rate is high.
Example 2
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.98:4:0.02:0.01:1.02O3、Al2O3、CeO2、Sm2O3And Ga2O3Obtaining (Y)2.98Ce0.01Sm0.01)(Al4.0Ga1.0)O12A ceramic material.
When the ceramic material obtained in example 2 of the present invention was tested by the test method of example 1, the ceramic material obtained in example 2 of the present invention had a transmittance of 75% at a wavelength of 500nm or more, was a transparent ceramic, had a thermal conductivity of 8.7W/m · K, had emission intensities of 1, 0.99, 0.956, 0.932, and 0.907 at 25 ℃, 50 ℃, 100 ℃, 150 ℃, and 200 ℃, respectively, had good thermal stability, and was able to emit green light having a peak position of 517nm under excitation of blue light, and had a high fluorescence conversion rate.
Example 3
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.994:4.4:0.006:0.003:0.5:0.22O3、Al2O3、CeO2、Pr2O3And Ga2O3And GeO2Obtaining (Y)2.994Ce0.003Pr0.003)(Al4.4Ga0.5Ge0.1)O12A ceramic material.
When the ceramic material obtained in example 3 of the present invention was tested by the test method of example 1, the ceramic material obtained in example 3 of the present invention showed a transmittance of 77% at a wavelength of 500nm or more, was a transparent ceramic, had a thermal conductivity of 8.1W/m · K, and had emission intensities of 1, 0.99, 0.959, 0.933, and 0.902 at 25 ℃, 50 ℃, 100 ℃, 150 ℃, and 200 ℃, respectively, and had good thermal stability, and was able to emit green light having a peak position of 520nm under excitation of blue light, and had a high fluorescence conversion rate.
Example 4
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.98:3.5:0.02:0.01:1:0.52O3、Al2O3、CeO2、Tb2O3Ga2O3And Sc2O3Obtaining (Y)2.98Ce0.01Tb0.01)(Al3.5GaSc0.5)O12A ceramic material.
According to the detection method in the embodiment 1, the ceramic material prepared in the embodiment 4 of the present invention is detected, and the detection result shows that the ceramic material prepared in the embodiment 4 of the present invention is transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 513nm under the excitation of blue light, and has a high fluorescence conversion rate.
Example 5
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.96:3.5:0.02:0.03:1:0.52O3、Al2O3、CeO2、Dy2O3、Ga2O3And V2O5Obtaining (Y)2.96Ce0.01Dy0.03)(Al3.5GaV0.5)O12A ceramic material.
According to the detection method of the embodiment 1, the ceramic material prepared in the embodiment 5 of the present invention is detected, and the detection result shows that the ceramic material prepared in the embodiment 5 of the present invention has a transmittance of 75% for transmitting a wavelength of 500nm or more, is a transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 511nm under the excitation of blue light, and has a high fluorescence conversion rate.
Example 6
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.91:3.5:0.06:0.03:0.03:1.52O3、Al2O3、CeO2、Lu2O3、La2O3And Ga2O3Obtaining (Y)2.91Ce0.03La0.03Lu0.03)(Al3.5Ga1.5)O12A ceramic material.
According to the detection method of the embodiment 1, the ceramic material prepared in the embodiment 6 of the present invention is detected, and the detection result shows that the ceramic material prepared in the embodiment 6 of the present invention has a transmittance of 72% for transmitting a wavelength of 500nm or more, is a transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 512nm under the excitation of blue light, and has a high fluorescence conversion rate.
Example 7
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.91:3:0.12:0.03:22O3、Al2O3、CeO2、Pr2O3And Ga2O3Obtaining (Y)2.91Ce0.06Pr0.03)(Al3Ga2)O12A ceramic material.
According to the detection method of the embodiment 1, the ceramic material prepared in the embodiment 7 of the present invention is detected, and the detection result shows that the ceramic material prepared in the embodiment 7 of the present invention is transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 511nm under the excitation of blue light, and has high fluorescence conversion rate.
Example 8
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high purity was weighed in a molar ratio of 2.88:4.5:0.12:0.06:0.4:0.2Y2O3、Al2O3、CeO2、Pr2O3、Ga2O3And SiO2Obtaining (Y)2.88Ce0.06Pr0.06)(Al4.5Ga0.4Si0.1)O12A ceramic material.
According to the detection method of the embodiment 1, the ceramic material prepared in the embodiment 8 is detected, and the detection result shows that the ceramic material prepared in the embodiment 8 is transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 519nm under the excitation of blue light, and has high fluorescence conversion rate.
Example 9
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.91:4.5:0.12:0.03:0.3:0.22O3、Al2O3、CeO2、Pr2O3、Ga2O3And Sc2O3Obtaining (Y)2.91Ce0.06Pr0.03)(Al4.5Ga0.3Sc0.2)O12A ceramic material.
The ceramic material prepared in the embodiment 9 of the present invention is detected according to the detection method in the embodiment 1, and the detection result shows that the ceramic material prepared in the embodiment 9 of the present invention is transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 522nm under the excitation of blue light, and has a high fluorescence conversion rate.
Example 10
A ceramic material was prepared as described in example 1, except that, in contrast to example 1, the desired high-purity Y was weighed in a molar ratio of 2.88:4.5:0.12:0.06:0.4:0.12O3、Al2O3、CeO2、Pr2O3、Ga2O3And V2O5Obtaining (Y)2.88Ce0.06Pr0.06)(Al4.5Ga0.4V0.1)O12A ceramic material.
The ceramic material prepared in the embodiment 10 of the present invention is detected according to the detection method in the embodiment 1, and the detection result shows that the ceramic material prepared in the embodiment 10 of the present invention is transparent ceramic, has good thermal conductivity and thermal stability, can emit green light with a peak position of 521nm under the excitation of blue light, and has a high fluorescence conversion rate.
Example 11
A ceramic material was prepared as in example 1, except that the desired high-purity Y was weighed in a molar ratio of 2.999:4.95:0.002:0.05 as in example 12O3、Al2O3、CeO2And Ga2O3Obtaining (Y)2.999Ce0.001)(Al4.95Ga0.05)O12A ceramic material.
When the ceramic material obtained in example 11 of the present invention was tested by the test method of example 1, the ceramic material obtained in example 11 of the present invention showed 78% transmittance at a wavelength of 500nm or more, was a transparent ceramic, had 11.8W/m · K thermal conductivity, had 1, 0.994, 0.965, 0.946, and 0.915 light intensities at 25 ℃, 50 ℃, 100 ℃, 150 ℃, and 200 ℃, respectively, and had good thermal stability, and was able to emit green light with a peak position of 525nm under excitation of blue light, and had a high fluorescence conversion ratio.
As can be seen from the above examples, the present invention provides a ceramic material consisting of Y2O3、Al2O3、CeO2The oxide of R and the oxide of M; r is selected from one or more of La, Pr, Sm, Tb, Dy and Lu; and M is selected from one or more of Si, Ge, Ga, Sc and V. The ceramic material provided by the invention is Ce3+The active ion is the main active ion, the M ion is doped or the M and R ions are simultaneously doped to adjust the luminous peak position of the ceramic material, so that the ceramic material can generate green light with the peak wavelength less than or equal to 525nm and the luminous peak half-width height less than or equal to 70nm under the excitation of blue laser, the transparency of the ceramic material can be adjusted through the porosity, and the ceramic material has good color performance. The ceramic material has good thermal conductivity and thermal stability, and can be prepared into fluorescent ceramic devices,the fluorescent powder can be replaced for the projection system, the heat fading of the luminous brightness when the fluorescent powder is adopted is effectively avoided, the projection system has good color performance, ultra-long service life and good stability, and the output brightness of the system is improved to the maximum extent.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
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 (9)
1. A ceramic material consisting of2O3、Al2O3、CeO2And M oxide;
the M is selected from one or more of Si, Ge, Ga, Sc and V;
the preparation raw materials of the ceramic material also comprise an oxide of R, wherein the R is selected from one or more of La, Pr, Sm, Tb, Dy and Lu;
the molar ratio of Y, Ce, R, Al and M in the ceramic material is (3-x-Y): x: y (5-z): z;
0.001≤x≤0.06；
0≤y≤0.06；
0.05≤z≤2。
2. a process for the preparation of the ceramic material according to claim 1, comprising the steps of:
(1) will Y2O3、Al2O3、CeO2Mixing the oxide of M and the oxide of R to prepare a powder raw material;
(2) pressing and molding the powder raw material to obtain a green body;
(3) and sintering the green body to obtain the ceramic material.
3. The method as claimed in claim 2, wherein the pressure during the step (2) press forming is 200MPa or more.
4. The method of claim 2, wherein the step (2) press forming is cold isostatic pressing.
5. The method according to claim 2, wherein the sintering temperature in the step (3) is 1400-1750 ℃.
6. The method according to claim 2, wherein the sintering time in the step (3) is 5-20 hours.
7. The method according to claim 2, wherein the step (3) sintering is sintering under vacuum;
vacuum degree of not less than 3 × 10-3Pa。
8. The method according to claim 2, wherein the step (3) sintering is sintering under an oxygen atmosphere;
the pressure of oxygen is 0.01 to 0.1 MPa.
9. A fluorescent ceramic device comprising the ceramic material of claim 1.
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