CN112661512A - Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature - Google Patents
Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature Download PDFInfo
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- CN112661512A CN112661512A CN202011536263.6A CN202011536263A CN112661512A CN 112661512 A CN112661512 A CN 112661512A CN 202011536263 A CN202011536263 A CN 202011536263A CN 112661512 A CN112661512 A CN 112661512A
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- 239000000843 powder Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 25
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052574 oxide ceramic Inorganic materials 0.000 title claims abstract description 7
- 239000011224 oxide ceramic Substances 0.000 title claims abstract description 7
- 238000000280 densification Methods 0.000 title claims description 10
- 239000000919 ceramic Substances 0.000 claims abstract description 29
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 38
- 239000011812 mixed powder Substances 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 25
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 16
- 229910003564 SiAlON Inorganic materials 0.000 claims description 14
- 239000004677 Nylon Substances 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 10
- 229920001778 nylon Polymers 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000003826 uniaxial pressing Methods 0.000 claims description 6
- 239000012190 activator Substances 0.000 claims 2
- 238000003801 milling Methods 0.000 claims 1
- 238000004020 luminiscence type Methods 0.000 abstract description 6
- 238000000498 ball milling Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 239000008188 pellet Substances 0.000 description 12
- 238000005245 sintering Methods 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
A method for densifying fluorescent powder and yttrium oxide ceramic at room temperature belongs to the technical field of preparation and application of fluorescent powder ceramic materials. The commercial fluorescent powder and the yttrium oxide are compacted at room temperature by fine ball milling and twice cold isostatic pressing and adding deionized water before the second cold isostatic pressing. The relative density of the prepared fluorescent powder ceramic reaches 53-58% at room temperature, and the prepared fluorescent powder ceramic has no influence on the luminescence of the fluorescent powder. The preparation method provided by the invention has the advantages of simple process and stable product performance, and is suitable for industrial production.
Description
Technical Field
The invention provides a method for densifying fluorescent powder and yttrium oxide ceramic at room temperature, belonging to the technical field of preparation and application of fluorescent powder ceramic materials.
Background
As the demand for high power semiconductor lighting increases, the substrates used for dispersing phosphor particles are currently resins, glasses, silica gels, and the like. However, these materials have low thermal conductivity and cause thermal degradation, and are not suitable for use at high power. Therefore, fluorescent conversion materials have been developed using ceramics. For example, YAG Ce3+The thermal conductivity of the ceramic is about 8Wm-1K-1. Generally, high densification of ceramics requires high temperature sintering, which degrades and alters the phosphor particles. Therefore, high temperature sintering should be avoided and normal temperature densification is desired.
Both hydrothermal hot pressing and cold sintering methods reported in the past are ceramic densification methods that do not use high temperatures. The non-sintering method adopts mechanically activated particle surface, SiO at room temperature2Has reached a density of 2.05 g/cm3. The hydrothermal hot pressing method is a method of mechanically densifying a sample by applying pressure with a piston under hydrothermal conditions. The hydrothermal hot pressing method can realize the densification of the glass at a low temperature of 260 ℃. The cold sintering method is a method in which a liquid and a powder are mixed, a pressure of several hundred MPa is applied, the mixture is heated in a uniaxial mold, and mass transfer is accelerated by a liquid phase to densify the material. At 126 ℃, the relative density value of the ZnO ceramic reaches over 90 percent. However, uniaxial pressing introduces anisotropic particle packing due to the stress distribution that occurs in the powder layer.
Disclosure of Invention
1. In order to solve the problems, the invention provides a method for densifying fluorescent powder and yttrium oxide ceramic at room temperature. The relative density of the prepared fluorescent powder ceramic reaches 53-58% at room temperature, and the prepared fluorescent powder ceramic has no influence on the luminescence of the fluorescent powder. Comprises the following steps:
using Y with a purity of more than 99.9%2O3Powder as raw material, Y2O3The powder raw material comprises powder A, B or mixed powder of A and B, wherein the average particle size of the powder A is 0.2-0.3 mu m, the average particle size of the powder B is 0.4-0.5 mu m, and the mass ratio of the powder A to the powder B is 0: 100-100: 0; mixing fluorescent powder particles with Y2O3Mixing the powder, the fluorescent powder and Y2O3The mass ratio of the powder is 0.5-2: 1, wrapping the zirconia balls with the diameter of 5-10 mm by using nylon cloth, and adding the nylon cloth to the fluorescent powder and the Y2O3Mixing, wherein the mass fraction of the zirconia globules is 20-30% of the mixed powder; then, ball-milling the mixed powder for 1-3 minutes by using a planetary ball mill at 1800-2200 rpm; injecting the powder into a die, performing uniaxial pressing for 30-60 seconds at 50-70 MPa by using a press, and performing primary cold isostatic pressing for 1-3 minutes at room temperature at 900-1000 MPa to form a blank; and then, adding deionized water accounting for 7-9% of the mass of the green body into the green body at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 900-1000 MPa, and the pressure maintaining time is 1-2 h, so as to finally obtain the ceramic with compact fluorescent powder and yttrium oxide.
Advantageous effects
1. The prepared fluorescent powder ceramic is successfully compact at room temperature, the relative density of the prepared fluorescent powder ceramic reaches 53-58% at room temperature, and the prepared fluorescent powder ceramic has no influence on the luminescence of the fluorescent powder.
2. In the process of preparing the fluorescent powder ceramic, the method selects high-purity raw material powder, strictly controls the introduction of impurities, and is very suitable for preparing the fluorescent powder ceramic.
3. The preparation method of the fluorescent powder ceramic provided by the invention has the advantages of high yield and productivity, simple preparation process and no strict requirements on preparation time arrangement, can effectively improve the yield and reduce the production cost, and is very suitable for industrial production.
Drawings
FIG. 1 is a relative density curve of green bodies prepared in examples 1-5 after uniaxial pressing and cold isostatic pressing, as a function of the mass fraction of powder A;
FIG. 2 is a graph showing the emission spectra of examples 1 and 6.
Detailed Description
The present invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention.
Example 1: eu, alpha-SiAlON2+Phosphor and Y2O3Is dense
Adopting Y with the average grain diameter of 0.2-0.3 mu m and the purity of more than 99.9%2O3The powder is used as a raw material. Mixing alpha-SiAlON with Eu2+Phosphor powder particles and Y2O3Mixing the powder, fluorescent powder and mixed Y2O3The mass ratio of the powder is 2: 1, wrapping zirconia pellets with the diameter of 5mm by using nylon cloth, wherein the mass fraction of the zirconia pellets is 30% of that of the mixed powder, adding the zirconia pellets into the mixed powder, and then ball-milling the mixed powder for 1 minute at 2200rpm by using a planetary ball mill. The powder was injected into a mold, uniaxially pressed at 70MPa for 30 seconds, and then preliminarily cold-isostatically pressed at 1000MPa for 1 minute at room temperature. And then, adding deionized water accounting for 9% of the mass of the blank into the blank at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 900MPa, and the pressure maintaining time is 2 h. Finally obtaining the ceramic with compact fluorescent powder and yttrium oxide.
Example 2: eu, alpha-SiAlON2+Phosphor and Y2O3Is dense
Adopting Y with the purity of more than 99.9 percent and the average grain diameter of 0.4-0.5 mu m2O3The powder is used as a raw material. Mixing alpha-SiAlON with Eu2+Phosphor powder particles and Y2O3Mixing the powder, fluorescent powder and mixed Y2O3The mass ratio of the powder is 0.5: and 1, wrapping zirconia balls with the diameter of 10mm by using nylon cloth, wherein the mass fraction of the zirconia balls is 20-30% of the mixed powder, adding the zirconia balls into the mixed powder, and then ball-milling the mixed powder for 3 minutes by using a planetary ball mill at 1800 rpm. The powder was injected into a mold, uniaxially pressed at 50MPa for 60 seconds, and then placed in a chamberPreliminary cold isostatic pressing was carried out at 900MPa for 3 minutes at room temperature. And then, adding deionized water accounting for 7% of the mass of the blank into the blank at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 1000MPa, and the pressure maintaining time is 1 h. Finally obtaining the ceramic with compact fluorescent powder and yttrium oxide.
Example 3: eu, alpha-SiAlON2+Phosphor and Y2O3Is dense
Using Y with two different average particle sizes and a purity of more than 99.9%2O3The powder is used as a raw material, wherein the average particle size of the powder A is 0.2-0.3 mu m, the average particle size of the powder B is 0.4-0.5 mu m, and the mass ratio of the powder A to the powder B is 30: 70. Mixing alpha-SiAlON with Eu2+Mixing fluorescent powder particles with A, B powder, and mixing fluorescent powder with mixed Y powder2O3The mass ratio of the powder is 0.8: 1, zirconia pellets having a diameter of 6mm were wrapped with nylon cloth, the mass fraction of the zirconia pellets was 25% of the mixed powder, and added to the mixed powder, and then the mixed powder was ball-milled for 2 minutes at 2000rpm using a planetary ball mill. The powder was injected into a mold, uniaxially pressed at 60MPa for 45 seconds, and then preliminarily cold-isostatically pressed at 950MPa for 2 minutes at room temperature. And then, adding deionized water accounting for 7-9% of the mass of the blank into the blank at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 980MPa, and the pressure maintaining time is 1.5 h. Finally obtaining the ceramic with compact fluorescent powder and yttrium oxide.
Example 4: eu, alpha-SiAlON2+Phosphor and Y2O3Is dense
Using Y with two different average particle sizes and a purity of more than 99.9%2O3The powder is used as a raw material, wherein the average particle size of the powder A is 0.2-0.3 mu m, the average particle size of the powder B is 0.4-0.5 mu m, and the mass ratio of the powder A to the powder B is 70: 30. Mixing alpha-SiAlON with Eu2+Mixing fluorescent powder particles with A, B powder, and mixing fluorescent powder with mixed Y powder2O3The mass ratio of the powder is 0.8: 1, zirconia pellets having a diameter of 6mm were wrapped with nylon cloth, the mass fraction of the zirconia pellets was 25% of the mixed powder, and added to the mixed powder, and then the mixed powder was ball-milled for 2 minutes at 2000rpm using a planetary ball mill. Injecting the powder into a mold, and uniaxially pressing at 60MPaPressing for 45 seconds, and then preliminary cold isostatic pressing at 950MPa for 2 minutes at room temperature. And then, adding deionized water accounting for 7-9% of the mass of the blank into the blank at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 980MPa, and the pressure maintaining time is 1.5 h. Finally obtaining the ceramic with compact fluorescent powder and yttrium oxide.
Example 5: eu, alpha-SiAlON2+Phosphor and Y2O3Is dense
Using Y with two different average particle sizes and a purity of more than 99.9%2O3The powder is used as a raw material, wherein the average particle size of the powder A is 0.2-0.3 mu m, the average particle size of the powder B is 0.4-0.5 mu m, and the mass ratio of the powder A to the powder B is 50: 50. Mixing alpha-SiAlON with Eu2+Mixing fluorescent powder particles with A, B powder, and mixing fluorescent powder with mixed Y powder2O3The mass ratio of the powder is 0.8: 1, zirconia pellets having a diameter of 6mm were wrapped with nylon cloth, the mass fraction of the zirconia pellets was 25% of the mixed powder, and added to the mixed powder, and then the mixed powder was ball-milled for 2 minutes at 2000rpm using a planetary ball mill. The powder was injected into a mold, uniaxially pressed at 60MPa for 45 seconds, and then preliminarily cold-isostatically pressed at 950MPa for 2 minutes at room temperature. And then, adding deionized water accounting for 7-9% of the mass of the blank into the blank at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 980MPa, and the pressure maintaining time is 1.5 h. Finally obtaining the ceramic with compact fluorescent powder and yttrium oxide.
Example 6: beta-SiAlON Eu2+Phosphor and Y2O3Is dense
Adopting Y with the average grain diameter of 0.2-0.3 mu m and the purity of more than 99.9%2O3The powder is used as a raw material. beta-SiAlON: Eu2+Phosphor powder particles and Y2O3Mixing the powder, fluorescent powder and mixed Y2O3The mass ratio of the powder is 2: 1, wrapping zirconia pellets with the diameter of 5mm by using nylon cloth, wherein the mass fraction of the zirconia pellets is 30% of that of the mixed powder, adding the zirconia pellets into the mixed powder, and then ball-milling the mixed powder for 1 minute at 2200rpm by using a planetary ball mill. Injecting the powder into a mold, performing uniaxial pressing at 70MPa for 30 s, and performing primary cooling at 1000MPa at room temperaturePressing for 1 minute. And then, adding deionized water accounting for 9% of the mass of the blank into the blank at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 900MPa, and the pressure maintaining time is 2 h. Finally obtaining the ceramic with compact fluorescent powder and yttrium oxide.
As can be seen from the XRD spectrum in figure 1, the method (examples 1-5) provided by the invention successfully compacts the fluorescent powder and the yttrium oxide at room temperature, and the relative density of the compacted ceramic is tested by adopting the national standard GB/T3810.3-2006, so that the relative density of the prepared fluorescent powder ceramic reaches 53-58% at room temperature, and the relative density of the green body after water cooling and the like is improved by 5-8% compared with that of the green body after uniaxial pressing, which means that the method provided by the invention realizes the densification of the green body only at room temperature, has mild preparation conditions, reduces the energy consumption, and is suitable for large-scale industrial production. Taking example 1 and example 6 as examples, according to the comparison of the luminescence curves of the ceramic densified by the method provided by the present invention and the two phosphors not densified in fig. 2, the method provided by the present invention for densification hardly affects the luminescence of the phosphors, which shows that the densification method provided by the present invention can retain the original luminescence property of the phosphors, and is more dense (reduces air holes) at the same time, thereby enhancing the thermal conductivity, and has a smaller volume, so that the LED device has a flexible design space, and can be applied to products such as LED devices, especially to high-power LED devices.
Claims (4)
1. A method for densifying fluorescent powder and yttrium oxide ceramic at room temperature is characterized in that the fluorescent powder and the ceramic are densified together at room temperature, and the method comprises the following specific steps:
using Y with a purity of more than 99.9%2O3Taking the powder as a raw material; mixing fluorescent powder particles with Y2O3Mixing the powder, the fluorescent powder and Y2O3The mass ratio of the powder is 0.5-2: 1, wrapping the zirconia balls with the diameter of 5-10 mm by using nylon cloth, and adding the nylon cloth to the fluorescent powder and the Y2O3The mass fraction of the zirconia globules is 20-30% of the mixed powder; then use the rowBall-milling the mixed powder for 1-3 minutes by using a star ball mill at 1800-2200 rpm; injecting the mixed powder into a mold, performing uniaxial pressing for 30-60 seconds at 50-70 MPa by using a press, and performing primary cold isostatic pressing for 1-3 minutes at room temperature at 900-1000 MPa to form a blank; and then, adding deionized water accounting for 7-9% of the mass of the green body into the green body at room temperature, and carrying out cold isostatic pressing again, wherein the pressure is 900-1000 MPa, and the pressure maintaining time is 1-2 h, so as to finally obtain the ceramic with compact fluorescent powder and yttrium oxide.
2. The method of claim 1, wherein Y is a Y-site activator, and Y is a Y-site activator2O3The powder is powder A or powder B or a mixed powder of powder A and powder B, wherein the mass ratio of the powder A to the powder B in the mixed powder of powder A and powder B is 0: 100-100: 0; the average particle size of the powder A is 0.2-0.3 μm, and the average particle size of the powder B is 0.4-0.5 μm.
3. The method for densification of phosphor and yttria ceramic at room temperature of claim 1, wherein the phosphor is α -SiAlON Eu2+Phosphor or beta-SiAlON: Eu2+And (3) fluorescent powder.
4. The room-temperature phosphor and yttrium oxide ceramic is characterized by being prepared by the preparation method of claim 1, wherein the relative density of the prepared phosphor ceramic reaches 53-58%.
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2020
- 2020-12-23 CN CN202011536263.6A patent/CN112661512A/en active Pending
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Application publication date: 20210416 |