CN114044668A - Cerium-doped yttrium aluminum garnet transparent ceramic raw material and preparation method thereof - Google Patents
Cerium-doped yttrium aluminum garnet transparent ceramic raw material and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 81
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 title claims abstract description 33
- 239000002994 raw material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 128
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 33
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 238000005469 granulation Methods 0.000 claims abstract description 22
- 230000003179 granulation Effects 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 16
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 16
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 16
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims abstract description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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 12
- 239000007921 spray Substances 0.000 claims abstract description 12
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 37
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims description 33
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 29
- 239000003153 chemical reaction reagent Substances 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 14
- 235000006408 oxalic acid Nutrition 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- 229960001759 cerium oxalate Drugs 0.000 claims description 5
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000004677 Nylon Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 13
- 238000009388 chemical precipitation Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 6
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 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 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The application relates to a cerium-doped yttrium aluminum garnet transparent ceramic raw material and a preparation method thereof. The raw materials comprise the following components in percentage by mass: 54-57% yttrium oxide powder; 40% -42% of alumina powder; 0-0.5% cerium oxide powder; 0-0.5% magnesium oxide powder; 0-0.5% of ethyl orthosilicate; 0-1% of PEG200 powder; 1-2% PVA. The preparation method comprises the following steps: mixing yttrium oxide powder, alumina powder, cerium oxide powder, magnesium oxide powder, ethyl orthosilicate and PEG200 powder together, and performing ball milling to obtain slurry; uniformly mixing the slurry and PVA, and adding the mixture into a granulation tower for spray granulation to obtain granulation powder; adding the granulated powder into a mold, and performing cold isostatic pressing after dry pressing to obtain a green body; pre-sintering the green body, sintering the green body under a vacuum condition, and then cooling and annealing to obtain the transparent ceramic, wherein the density of the transparent ceramic is close to a theoretical value of 4.55g/cm3, and the linear transmittance in a visible light range is higher than 74%.
Description
Technical Field
The application relates to transparent ceramic, in particular to a cerium-doped yttrium aluminum garnet transparent ceramic raw material and a preparation method thereof.
Background
The white light LED as a novel all-solid-state lighting source has the advantages of energy conservation, no pollution and the like, so that the white light LED has wide application prospect and market. The mainstream mode of the white light LED product sold in the current market is the combination mode of blue light LED and yellow fluorescent powder, and yttrium aluminum garnet Y3Al5O12YAG has the advantages of high-intensity radiation resistance and electron bombardment resistance, and is widely used as a luminescent matrix material, so cerium-doped yttrium aluminum garnet (Ce: YAG) is the preferred yellow fluorescent powder for preparing white LEDs.
In carrying out the present application, applicants have found that when white LEDs are currently being fabricated, Ce: YAG yellow fluorescent powder and epoxy resin or silica gel are mixed and coated on a blue LED chip according to a certain proportion, and the packaging method has the problems of low fluorescence conversion efficiency, easy aging, uneven luminosity and the like.
Disclosure of Invention
The embodiment of the application provides a cerium-doped yttrium aluminum garnet transparent ceramic raw material and a preparation method thereof, and solves the problems of low fluorescence conversion efficiency, easy aging, uneven luminosity and the like existing in the conventional process of preparing a white light LED.
In order to solve the above technical problem, the present application is implemented as follows:
in a first aspect, a cerium-doped yttrium aluminum garnet transparent ceramic raw material is provided, which comprises the following components in percentage by mass: 54-57% yttrium oxide powder; 40% -42% of alumina powder; 0-0.5% cerium oxide powder; 0-0.5% magnesium oxide powder; 0-0.5% of ethyl orthosilicate; 0-1% of PEG200 powder; 1-2% PVA.
In a first possible implementation manner of the first aspect, the yttrium oxide powder, the aluminum oxide powder and the magnesium oxide powder have a particle size of 0.5 to 2.0 μm and a purity of 99.9% or more, respectively.
In a second possible implementation manner of the first aspect, the preparation method of the cerium oxide powder includes the steps of: adding an oxalic acid reagent into the cerous nitrate analytical reagent, and adjusting the pH value of the cerous nitrate analytical reagent; adding excessive ammonia water into a cerium nitrate analytical reagent to precipitate cerium oxalate generated by the cerium nitrate and oxalic acid; after suction filtration, water washing and alcohol washing, the obtained precipitate is dried and calcined to obtain high-purity cerium oxide powder.
In combination with the second possible implementation manner of the first aspect, in a third possible implementation manner of the first aspect, the PH of the cerium nitrate analytical reagent is adjusted to 2.
With reference to the second possible implementation manner of the first aspect, in a fourth possible implementation manner of the first aspect, the calcination temperature of the precipitate is 1000-.
In a second aspect, a method for preparing a cerium-doped yttrium aluminum garnet transparent ceramic is provided, which comprises the following steps: weighing any one of the above-mentioned cerium-doped yttrium aluminum garnet transparent ceramic raw materials in the first aspect; mixing yttrium oxide powder, alumina powder, cerium oxide powder, magnesium oxide powder, ethyl orthosilicate and PEG200 powder together, and performing ball milling to obtain slurry; uniformly mixing the slurry and PVA, and adding the mixture into a granulation tower for spray granulation to obtain granulation powder; adding the granulated powder into a mold, and performing cold isostatic pressing after dry pressing to obtain a green body; pre-sintering the green body, sintering under vacuum condition, cooling and annealing to obtain the transparent ceramic.
In a first possible implementation manner of the second aspect, during ball milling, yttrium oxide powder, aluminum oxide powder, cerium oxide powder, magnesium oxide powder, ethyl orthosilicate and PEG200 powder are placed in a nylon ball milling tank, absolute ethyl alcohol is used as a ball milling medium, and alumina balls are used for ball milling for 10-12 hours on a planetary ball mill to obtain a uniformly mixed slurry.
In a second possible implementation manner of the second aspect, during spray granulation, after mixing the slurry with PVA, ethanol is used for dilution, so as to reduce the solid content to 30-35%, the air inlet temperature of the granulation tower is 80-110 ℃, the air outlet temperature is 60-100 ℃, the spray pressure is 0.05MPa-0.5MPa, and the particle size of the granulated powder is controlled to 50-80 μm.
In a third possible implementation manner of the second aspect, the pressure of the dry-pressing is 20 MPa; the pressure of the cold isostatic pressing is 150-200MPa, and the pressure maintaining time is 0.5-5 min; the presintering temperature of the green body is 1000 ℃, and the time is 8 h.
In a fourth possible implementation manner of the second aspect, when sintering and cooling annealing are performed on the green body under the vacuum condition, the temperature is raised to 1300 ℃ at the speed of 5-10 ℃/min, the temperature is kept for 60-100min, then the temperature is raised to 1780 ℃ at the speed of 2 ℃/min, the temperature is kept for 8-10h, then the temperature is lowered to 150 ℃ at the speed of 10 ℃/min, and then furnace cooling is performed, and then annealing is performed in 1450 ℃ air for 10 h.
Compared with the prior art, the application has the advantages that:
according to the cerium-doped yttrium aluminum garnet transparent ceramic raw material and the preparation method, the yellow transparent ceramic with excellent optical quality is prepared by regulating and controlling the components and the content of each component in the ceramic material, the ceramic density is close to the theoretical value of 4.55g/cm3, no air holes, impurities and second phases exist, the linear transmittance in a visible light range is higher than 74%, and the prepared transparent ceramic sample is suitable for being used as a high-efficiency packaging material of a white light LED.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a flow chart illustrating the steps of a method for preparing a cerium-doped yttrium aluminum garnet transparent ceramic according to an embodiment of the present application.
Detailed Description
For white light LED, the mainstream mode at present is the combination mode of blue light LED and yellow fluorescent powder, and yttrium aluminum garnet Y3Al5O12YAG (YAG for short) has the advantages of high-intensity irradiation resistance and electron bombardment resistance, and is widely used as a luminescent matrix material, so cerium-doped yttrium aluminum garnet (Ce: YAG) is the first choice of yellow fluorescent powder for preparing white LEDs, namely Ce: YAG yellow fluorescent powder and epoxy resin or silica gel are mixed and coated on a blue LED chip according to a certain proportion, however, the packaging method has the problems of low fluorescence conversion efficiency, easy aging, uneven luminosity and the like.
The transparent ceramic is a new optical functional material which is widely concerned in the present year, yttrium aluminum garnet (Y)3Al5O12YAG) as an ideal matrix for preparing transparent ceramics, has an isotropic cubic crystal structure, can reduce the scattering of incident light, and has excellent mechanical, thermal and mechanical properties. Ce3+Has 4f5d electronic configuration, is an activating ion with higher fluorescence efficiency in rare earth ions, so Ce is adopted3+Doped YAG transparent ceramics to replace Ce: the YAG fluorescent powder can avoid the use of epoxy resin and other packaging materials, and has good heat dissipation, good thermal stability and longer service life.
Meanwhile, the transparent ceramic can realize high doping concentration and high chemical uniformity, thereby improving the luminous efficiency, optical uniformity and stability of the white light LED device. In addition, in terms of the ceramic preparation process, Ce: the YAG transparent ceramic has short preparation period and low cost, is easy to prepare into various shapes and easy to integrate and package, and is expected to be widely applied to the field of white light LEDs.
Therefore, the cerium-doped yttrium aluminum garnet transparent ceramic raw material and the preparation method thereof adopt a raw material chemical precipitation method, a solid-phase reaction method and a vacuum sintering technology to prepare the Ce: YAG transparent ceramic, suitable for high efficiency white LED packaging material.
To make the objects, technical solutions and advantages of the present application more clear, embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Example 1
Please refer to fig. 1, which is a schematic flow chart illustrating steps of a method for preparing a cerium-doped yttrium aluminum garnet transparent ceramic according to an embodiment of the present application. As shown in the figure, the method 1 for preparing the cerium-doped yttrium aluminum garnet transparent ceramic is to prepare the YAG ceramic doped with 0.5 at% Ce. The preparation method 1 of the cerium-doped yttrium aluminum garnet transparent ceramic comprises the following steps 101 to 105, wherein:
Specifically, a cerium nitrate analytically pure reagent is used as a raw material, an oxalic acid reagent is used as an acidity adjusting reagent, in other words, the oxalic acid reagent is added into the cerium nitrate analytically pure reagent, the pH value of the cerium nitrate analytically pure reagent is adjusted to 2, ammonia water is added to precipitate cerium oxalate, the ammonia water is slightly excessive, the curing time is prolonged to 12 hours, suction filtration is carried out after curing is completed, the precipitate after suction filtration is washed with water for 3 times and washed with alcohol for 2 times, the obtained precipitate is dried in an oven at 80 ℃ for 60min, and then the dried precipitate is placed in a high-temperature furnace to be calcined at about 1100 ℃, so that high-purity cerium oxide powder is obtained.
And 102, mixing materials and carrying out ball milling. 360g of yttrium oxide powder, 272.28g of alumina powder, 2.76g of cerium oxide powder, 0.65g of magnesium oxide powder, 3.25g of ethyl orthosilicate and 5g of PEG200 powder were mixed together and ball-milled to obtain a slurry.
Specifically, 360g of yttrium oxide powder, 272.28g of alumina powder, 2.76g of cerium oxide powder, 0.65g of magnesium oxide powder, 3.25g of ethyl orthosilicate, 5g of PEG200 powder and 850g of absolute ethyl alcohol are added into a mixing container of a ball mill, and the mixing time, the rotating speed and the ball-to-material ratio of the ball mill are controlled to prepare uniformly dispersed slurry. In the above selected ceramic raw materials, except cerium oxide powder, the metal oxide powder has a particle size of (0.5-2.0) μm and a purity of not less than 99.9%, and is a commercial powder. Cerium oxide powder is used in a small amount, but the purity is critical, and it is prepared by the above-mentioned step 101 chemical precipitation method.
And 103, spraying and granulating. And uniformly mixing the slurry with 4g of PVA, and adding the mixture into a granulation tower for spray granulation to obtain granulated powder.
Specifically, absolute ethyl alcohol is added according to the original solid content of the slurry, the solid content is reduced to 35%, 4g of PVA is added to be uniformly mixed, magnetic stirring is used for dispersing for 2 hours, the slurry is sent to a centrifugal turntable nozzle of a spray granulator by a peristaltic pump, the rotating speed of the centrifugal turntable is 11000r/min, the inlet temperature is 110 ℃, the outlet temperature is 90 ℃, and the granulated powder with round particles and excellent flowing property is obtained.
And 104, molding. Adding the granulated powder into a mold, and carrying out cold isostatic pressing after dry pressing forming to obtain a green body.
Specifically, the granulation powder is placed in a mold, dry-pressing molding is carried out under the pressure of 20MPa, and then pressure is maintained in a cold isostatic pressing device under the pressure of 150 plus 200MPa for 0.5-5min, so as to obtain a green body.
And 105, sintering. Pre-sintering the green body, sintering under vacuum condition, cooling and annealing to obtain the transparent ceramic.
Specifically, the green body is placed in an air atmosphere high-temperature furnace for presintering at 1000 ℃ for 8h, then the green body is sintered at 1780 ℃ in a vacuum environment at high temperature, wherein the temperature is increased to 1300 ℃ at the speed of 5-10 ℃/min, the temperature is kept for 60-100min, then the temperature is increased to 1780 ℃ at the speed of 2 ℃/min, the temperature is kept for 8-10h, then the temperature is reduced to 150 ℃ at the speed of 10 ℃/min, the green body is cooled along with the furnace, and then the green body is annealed in 1450 ℃ air for 10h to obtain transparent ceramic, and the Ce: YAG transparent ceramics.
Test Ce: the YAG transparent ceramic has the following properties:
1. the Ce: YAG ceramic volume, weighing by using a precision balance, and then calculating according to a calculation formula of volume density to obtain Ce: the density of the YAG ceramic is 4.55g/cm3。
2. The visible light spectrum has no precise range, and the wavelength which can be sensed by human eyes is 400-760nm, so a spectrophotometer is adopted to test the 190-1100nm full-band transmittance, all data of 400-760nm are intercepted, the minimum value of the data is selected as the extreme value of the visible light transmittance, and the Ce: the visible light transmittance of the YAG ceramic is as high as 76%.
Example 2
Please refer to fig. 1, which is a schematic flow chart illustrating steps of a method for preparing a cerium-doped yttrium aluminum garnet transparent ceramic according to an embodiment of the present application. As shown in the figure, the method 1 for preparing the cerium-doped yttrium aluminum garnet transparent ceramic is to prepare the YAG ceramic doped with 0.5 at% Ce. The preparation method 1 of the cerium-doped yttrium aluminum garnet transparent ceramic comprises the following steps 101 to 105, wherein:
Specifically, a cerium nitrate analytically pure reagent is used as a raw material, an oxalic acid reagent is used as an acidity adjusting reagent, in other words, the oxalic acid reagent is added into the cerium nitrate analytically pure reagent, the pH value of the cerium nitrate analytically pure reagent is adjusted to 2, ammonia water is added to precipitate cerium oxalate, the ammonia water is slightly excessive, the curing time is prolonged to 12 hours, suction filtration is carried out after curing is completed, the precipitate after suction filtration is washed with water for 3 times and washed with alcohol for 2 times, the obtained precipitate is dried in an oven at 80 ℃ for 60min, and then the dried precipitate is placed in a high-temperature furnace to be calcined at about 1100 ℃, so that high-purity cerium oxide powder is obtained.
And 102, mixing materials and carrying out ball milling. 360g of yttrium oxide powder, 272.28g of alumina powder, 2.76g of cerium oxide powder, 0.65g of magnesium oxide powder, 5.04g of ethyl orthosilicate and 10g of PEG200 powder were mixed together and ball-milled to obtain a slurry.
Specifically, 360g of yttrium oxide powder, 272.28g of alumina powder, 2.76g of cerium oxide powder, 0.65g of magnesium oxide powder, 5.04g of ethyl orthosilicate, 10g of PEG200 powder and 800g of absolute ethyl alcohol are added into a mixing container of a ball mill, and the mixing time, the rotating speed and the ball-to-material ratio of the ball mill are controlled to prepare uniformly dispersed slurry. In the above selected ceramic raw materials, except cerium oxide powder, the metal oxide powder has a particle size of (0.5-2.0) μm and a purity of not less than 99.9%, and is a commercial powder. Cerium oxide powder is used in a small amount, but the purity is critical, and it is prepared by the above-mentioned step 101 chemical precipitation method.
And 103, spraying and granulating. And uniformly mixing the slurry with 3g of PVA, and adding the mixture into a granulation tower for spray granulation to obtain granulated powder.
Specifically, absolute ethyl alcohol is added according to the original solid content of the slurry, the solid content is reduced to 30%, then 3g of PVA is added and uniformly mixed, magnetic stirring is used for dispersing for 3h, the slurry is sent to a centrifugal turntable nozzle of a spray granulator by a peristaltic pump, the rotating speed of the centrifugal turntable is 11000r/min, the inlet temperature is 110 ℃, the outlet temperature is 90 ℃, and the granulated powder with round particles and excellent flowing property is obtained.
And 104, molding. Adding the granulated powder into a mold, and carrying out cold isostatic pressing after dry pressing forming to obtain a green body.
Specifically, the granulation powder is placed in a mold, dry-pressing molding is carried out under the pressure of 20MPa, and then pressure is maintained in a cold isostatic pressing device under the pressure of 150 plus 200MPa for 0.5-5min, so as to obtain a green body.
And 105, sintering. Pre-sintering the green body, sintering under vacuum condition, cooling and annealing to obtain the transparent ceramic.
Specifically, the green body is placed in an air atmosphere high-temperature furnace for presintering at 1000 ℃ for 8h, then the green body is sintered at 1780 ℃ in a vacuum environment at high temperature, wherein the temperature is increased to 1300 ℃ at the speed of 5-10 ℃/min, the temperature is kept for 60-100min, then the temperature is increased to 1780 ℃ at the speed of 2 ℃/min, the temperature is kept for 8-10h, then the temperature is reduced to 150 ℃ at the speed of 10 ℃/min, the green body is cooled along with the furnace, and then the green body is annealed in 1450 ℃ air for 10h to obtain transparent ceramic, and the Ce: YAG transparent ceramics.
Test Ce: the YAG transparent ceramic has the following properties:
1. the Ce: YAG ceramic volume, weighing by using a precision balance, and then calculating according to a calculation formula of volume density to obtain Ce: the density of the YAG ceramic is 4.55g/cm3。
2. The visible light spectrum has no precise range, and the wavelength which can be sensed by human eyes is 400-760nm, so a spectrophotometer is adopted to test the 190-1100nm full-band transmittance, all data of 400-760nm are intercepted, the minimum value of the data is selected as the extreme value of the visible light transmittance, and the Ce: the visible light transmittance of YAG ceramics is as high as 75 percent.
Example 3
Please refer to fig. 1, which is a schematic flow chart illustrating steps of a method for preparing a cerium-doped yttrium aluminum garnet transparent ceramic according to an embodiment of the present application. As shown in the figure, the method 1 for preparing the cerium-doped yttrium aluminum garnet transparent ceramic is to prepare the YAG ceramic doped with 0.2 at% Ce. The preparation method 1 of the cerium-doped yttrium aluminum garnet transparent ceramic comprises the following steps 101 to 105, wherein:
Specifically, a cerium nitrate analytically pure reagent is used as a raw material, an oxalic acid reagent is used as an acidity adjusting reagent, in other words, the oxalic acid reagent is added into the cerium nitrate analytically pure reagent, the pH value of the cerium nitrate analytically pure reagent is adjusted to 2, ammonia water is added to precipitate cerium oxalate, the ammonia water is slightly excessive, the curing time is prolonged to 12 hours, suction filtration is carried out after curing is completed, the precipitate after suction filtration is washed with water for 3 times and washed with alcohol for 2 times, the obtained precipitate is dried in an oven at 80 ℃ for 60min, and then the dried precipitate is placed in a high-temperature furnace to be calcined at about 1100 ℃, so that high-purity cerium oxide powder is obtained.
And 102, mixing materials and carrying out ball milling. 360g of yttrium oxide powder, 271.46g of alumina powder, 1.10g of cerium oxide powder, 0.63g of magnesium oxide powder, 3.25g of ethyl orthosilicate and 5g of PEG200 powder were mixed together and ball-milled to obtain a slurry.
Specifically, 360g of yttrium oxide powder, 271.46g of alumina powder, 1.10g of cerium oxide powder, 0.63g of magnesium oxide powder, 3.25g of ethyl orthosilicate, 5g of PEG200 powder and 850g of absolute ethyl alcohol are added into a mixing container of a ball mill, and the mixing time, the rotating speed and the ball-to-material ratio of the ball mill are controlled to prepare uniformly dispersed slurry. In the above selected ceramic raw materials, except cerium oxide powder, the metal oxide powder has a particle size of (0.5-2.0) μm and a purity of not less than 99.9%, and is a commercial powder. Cerium oxide powder is used in a small amount, but the purity is critical, and it is prepared by the above-mentioned step 101 chemical precipitation method.
And 103, spraying and granulating. And uniformly mixing the slurry with 3g of PVA, and adding the mixture into a granulation tower for spray granulation to obtain granulated powder.
Specifically, absolute ethyl alcohol is added according to the original solid content of the slurry, the solid content is reduced to 30%, then 3g of PVA is added and uniformly mixed, magnetic stirring is used for dispersing for 3h, the slurry is sent to a centrifugal turntable nozzle of a spray granulator by a peristaltic pump, the rotating speed of the centrifugal turntable is 11000r/min, the inlet temperature is 110 ℃, the outlet temperature is 90 ℃, and the granulated powder with round particles and excellent flowing property is obtained.
And 104, molding. Adding the granulated powder into a mold, and carrying out cold isostatic pressing after dry pressing forming to obtain a green body.
Specifically, the granulation powder is placed in a mold, dry-pressing molding is carried out under the pressure of 20MPa, and then pressure is maintained in a cold isostatic pressing device under the pressure of 150 plus 200MPa for 0.5-5min, so as to obtain a green body.
And 105, sintering. Pre-sintering the green body, sintering under vacuum condition, cooling and annealing to obtain the transparent ceramic.
Specifically, the green body is placed in an air atmosphere high-temperature furnace for presintering at 1000 ℃ for 8h, then the green body is sintered at 1780 ℃ in a vacuum environment at high temperature, wherein the temperature is increased to 1300 ℃ at the speed of 5-10 ℃/min, the temperature is kept for 60-100min, then the temperature is increased to 1780 ℃ at the speed of 2 ℃/min, the temperature is kept for 8-10h, then the temperature is reduced to 150 ℃ at the speed of 10 ℃/min, the green body is cooled along with the furnace, and then the green body is annealed in 1450 ℃ air for 10h to obtain transparent ceramic, and the Ce: YAG transparent ceramics.
Test Ce: the YAG transparent ceramic has the following properties:
1. the Ce: YAG ceramic volume, weighing by using a precision balance, and then calculating according to a calculation formula of volume density to obtain Ce: the density of the YAG ceramic is 4.55g/cm3。
2. The visible light spectrum has no precise range, and the wavelength which can be sensed by human eyes is 400-760nm, so a spectrophotometer is adopted to test the 190-1100nm full-band transmittance, all data of 400-760nm are intercepted, the minimum value of the data is selected as the extreme value of the visible light transmittance, and the Ce: the visible light transmittance of YAG ceramics is as high as 78%.
Combining Ce prepared in the above examples 1 to 3: the performance test result of the YAG transparent ceramic can be obtained, and the Ce: the density of the YAG transparent ceramic is 4.55g/cm3No air holes, impurities and second phase exist, and the visible light transmittance is higher than 74%.
In summary, the present application provides a cerium-doped yttrium aluminum garnet transparent ceramic raw material and a preparation method thereof. The yellow transparent ceramic with excellent optical quality is prepared by regulating and controlling the components and the content of each component in the ceramic material, the ceramic density is close to the theoretical value of 4.55g/cm3, no pores, impurities and second phases exist, the linear transmittance in a visible light range is higher than 74%, and the prepared transparent ceramic sample is suitable for being used as a high-efficiency packaging material of a white light LED.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The cerium-doped yttrium aluminum garnet transparent ceramic raw material is characterized by comprising the following components in percentage by mass:
54-57% yttrium oxide powder;
40% -42% of alumina powder;
0-0.5% cerium oxide powder;
0-0.5% magnesium oxide powder;
0-0.5% of ethyl orthosilicate;
0-1% of PEG200 powder;
1-2% PVA.
2. The raw material of cerium-doped yttrium aluminum garnet transparent ceramic as claimed in claim 1, wherein the particle sizes of the yttrium oxide powder, the aluminum oxide powder and the magnesium oxide powder are 0.5-2.0 μm respectively, and the purities thereof are respectively greater than or equal to 99.9%.
3. The cerium-doped yttrium aluminum garnet transparent ceramic raw material as claimed in claim 1, wherein the preparation method of the cerium oxide powder comprises the steps of:
adding an oxalic acid reagent into a cerous nitrate analytical reagent, and adjusting the pH value of the cerous nitrate analytical reagent;
adding excessive ammonia water into the cerium nitrate analytical reagent to precipitate cerium oxalate generated by the cerium nitrate and oxalic acid;
after suction filtration, water washing and alcohol washing, the obtained precipitate is dried and calcined to obtain high-purity cerium oxide powder.
4. The cerium-doped yttrium aluminum garnet transparent ceramic raw material as claimed in claim 3, wherein the pH value of the cerium nitrate analytical reagent is adjusted to 2.
5. The Ce-doped YAG transparent ceramic raw material as claimed in claim 3, wherein the temperature of the obtained precipitate is 80 ℃, the drying time is 60min, and the calcination temperature of the precipitate is 1000-.
6. A method for preparing cerium-doped yttrium aluminum garnet transparent ceramic is characterized by comprising the following steps:
weighing the raw material of the cerium-doped yttrium aluminum garnet transparent ceramic of any one of the claims 1 to 5;
mixing the yttrium oxide powder, the aluminum oxide powder, the cerium oxide powder, the magnesium oxide powder, the ethyl orthosilicate and the PEG200 powder together, and performing ball milling to obtain slurry;
uniformly mixing the slurry and the PVA, and adding the mixture into a granulation tower for spray granulation to obtain granulated powder;
adding the granulation powder into a mold, and performing cold isostatic pressing after dry pressing forming to obtain a green body;
pre-sintering the green body, sintering under a vacuum condition, and cooling and annealing to obtain the transparent ceramic.
7. The preparation method of the cerium-doped yttrium aluminum garnet transparent ceramic, according to claim 6, wherein during ball milling, the yttrium oxide powder, the aluminum oxide powder, the cerium oxide powder, the magnesium oxide powder, the ethyl orthosilicate and the PEG200 powder are placed in a nylon ball milling tank, absolute ethyl alcohol is used as a ball milling medium, and the aluminum oxide balls are used for ball milling for 10-12 hours in a planetary ball milling manner to obtain the uniformly mixed slurry.
8. The method for preparing the cerium-doped yttrium aluminum garnet transparent ceramic as claimed in claim 6, wherein during spray granulation, the slurry is diluted with ethanol after being mixed with the PVA, so as to reduce the solid content to 30-35%, the air inlet temperature of the granulation tower is set to 80-110 ℃, the air outlet temperature is set to 60-100 ℃, the spraying pressure is set to 0.05MPa-0.5MPa, and the particle size of the granulated powder is controlled to 50-80 μm.
9. The method for preparing the cerium-doped yttrium aluminum garnet transparent ceramic according to claim 6, wherein the pressure of the dry pressing is 20 MPa; the pressure of the cold isostatic pressing is 150-200MPa, and the pressure maintaining time is 0.5-5 min; the pre-sintering temperature of the green body is 1000 ℃, and the time is 8 h.
10. The method for preparing the cerium-doped yttrium aluminum garnet transparent ceramic according to claim 6, wherein the green body is sintered under vacuum condition and is annealed by cooling, the temperature is increased to 1300 ℃ at the speed of 5-10 ℃/min, the temperature is maintained for 60-100min, the temperature is increased to 1780 ℃ at the speed of 2 ℃/min, the temperature is maintained for 8-10h, the temperature is reduced to 150 ℃ at the speed of 10 ℃/min, the ceramic is cooled along with the furnace, and the ceramic is annealed in 1450 ℃ air for 10 h.
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