CN112573924A - Novel red fluorescent ceramic sheet and preparation method thereof - Google Patents
Novel red fluorescent ceramic sheet and preparation method thereof Download PDFInfo
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Abstract
A novel red fluorescent ceramic chip and a preparation method thereof belong to the technical field of luminescent material preparation and application. Chemical component is K2SiF6:xMn4+Wherein x is mass fraction, x is more than 0 and less than or equal to 0.01, the fluorescent ceramic sheet is prepared by hot pressing, and Mn is defined in the invention4+The concentration is lower doped, so that the light emitting loss in the up-conversion and temperature rise is reduced, and particularly, the thermal stability is greatly improved under higher luminous flux. The product provided by the invention has stable performance.
Description
Technical Field
The invention provides a novel red fluorescent ceramic chip and a preparation method thereof, belonging to the technical field of preparation and application of transparent ceramic materials.
Background
Commercial, residential, and other life and high performance requirements require illumination of white light emitting diodes (pc-LEDs) that are employing fluorescent conversion on a large scale. LEDs are replacing other lighting technologies due to their advantages of higher energy conversion efficiency, longer lifetime, low cost, and environmental friendliness. In pc-LEDs, blue emitting InGaN chips are commonly combined with one or more green-yellow cerium doped garnet phosphors, and a red phosphor, to display white light emission. Red phosphors for LED lighting have been the subject of recent research requiring strong absorption at 450nm and narrow emission around 630nm, while very low emission above 650nm is required for optimal emission performance.
LED packages typically coat the LED chip with phosphor, which works well for low to moderate blue light flux. However, for high drive applications, such as in automotive headlamps, monolithic translucent fluorescent ceramic sheets are typically used. The ceramic sheet helps to dissipate heat at higher thermal conductivity because thermal quenching reduces quantum efficiency at high temperatures. This is especially important in high luminous flux applications. The highly scattering phosphor material can only be designed with a short pump path length. The concentration of the activator cannot be reduced, further reducing the loss of concentration quenching and thermal quenching, thereby reducing the efficiency of high temperature and high light flux. Therefore, when a scene with high power is needed, the scattering inside the fluorescent powder needs to be reduced, and the fluorescent powder needs to be converted into a more compact material.
Disclosure of Invention
1. In order to solve the problems, the invention provides a novel red fluorescent ceramic chip and a preparation method thereof, wherein the chemical component is K2SiF6:xMn4+Wherein x is mass fraction, x is more than 0 and less than or equal to 0.01, the fluorescent ceramic sheet is prepared by hot pressing, and Mn is defined in the invention4+Doping at lower concentrations reduces the luminescence losses at up-conversion and temperature rise, especially at higher luminous fluxes.
2. The technical scheme of the invention is as follows:
first, K is synthesized2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO2Grinding and mixing the materials in an agate mortar, treating and heating the materials for 10 to 30 minutes under flowing HF gas at the temperature of 300 to 500 ℃, and repeating the treatment for 2 to 3 times. Then hot-pressing to prepare ceramic, adding K2SiF6:Mn4+The powder is put into a steel die and lined with graphite foil. Then the die is put into a uniaxial hot press, and the vacuum degree is less than 1 multiplied by 10 at 300-500 DEG C-6Pressing under 150-200 MPa in vacuum of Pa, and maintaining the pressure for 2-4 hours. And then slowly and uniformly releasing the pressure to normal pressure, and finally polishing the surface of the ceramic wafer to obtain the fluorescent ceramic wafer.
The invention has the beneficial effects that:
1. mn defined in the invention4+The fluorescent ceramic sheet prepared under the doping concentration reduces the light-emitting loss during up-conversion and temperature rise, and particularly improves the thermal stability under higher luminous flux;
2. in the process of preparing the fluorescent ceramic chip, the method selects high-purity raw material powder, strictly controls the introduction of impurities, and is very suitable for preparing the fluorescent ceramic chip.
Drawings
FIG. 1 is a picture of a fluorescent ceramic plate prepared in examples 1, 2, 3, 4 and 5;
FIG. 2 is a graph of emission spectra of fluorescent ceramic sheets with different doping concentrations prepared in examples 1, 2, 3, 4 and 5 under 450nm excitation;
a, B in FIG. 3 are the emission spectra within 300 ℃ for the fluorescent ceramic prepared in example 2 and the phosphor prepared in example 6, respectively.
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: k2SiF6: 0.45wt.%Mn4+Fluorescent ceramic plate
First, K is synthesized2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO2Grinding and mixing the materials in an agate mortar, respectively treating and heating the materials for 30 minutes under flowing HF gas at 300 ℃, and repeating the treatment for 2-3 times. Then hot pressing to prepare ceramic, adding K with different doping concentrations2SiF6:Mn4+The powder is respectively put into a steel die and lined with graphite foil. Then loading the mold into a uniaxial hot press with a vacuum degree of less than 1 × 10 at 500 deg.C-6Pressing under 175MPa in vacuum of Pa, maintaining the pressure for 4 hours, then uniformly releasing the pressure to normal pressure, and finally polishing the surfaces of the ceramic plates respectively to obtain the fluorescent ceramic plates.
Example 2: k2SiF6: 0.1wt.%Mn4+Fluorescent ceramic plate
First, K is synthesized2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO2Grinding and mixing the materials in an agate mortar, treating and heating the materials for 10 minutes under flowing HF gas at 500 ℃, and repeating the treatment for 2-3 times. Then hot-pressing to prepare ceramic, adding K2SiF6:Mn4+The powder is put into a steel die and lined with graphite foil. Then loading the mold into a uniaxial hot press with a vacuum degree of less than 1 × 10 at 300 deg.C-6Pressing under 150MPa in vacuum of Pa, maintaining the pressure for 2 hours, and then uniformly releasing the pressure to the normal pressure. And finally, polishing the surface of the ceramic wafer to obtain the fluorescent ceramic wafer.
Example 3: k2SiF6: 0.25wt.%Mn4+Fluorescent ceramic plate
First, K is synthesized2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO2Grinding and mixing in agate mortar at 350 deg.CThe treatment is carried out for 20 minutes under flowing HF gas, and the treatment is repeated for 2 to 3 times. Then hot-pressing to prepare ceramic, adding K2SiF6:Mn4+The powder is put into a steel die and lined with graphite foil. Then loading the mold into a uniaxial hot press with a vacuum degree of less than 1 × 10 at 400 deg.C-6Pressing under 200MPa in vacuum of Pa, maintaining the pressure for 3 hours, and then uniformly releasing the pressure to the normal pressure. And finally, polishing the surface of the ceramic wafer to obtain the fluorescent ceramic wafer.
Example 4: k2SiF6: 0.5wt.%Mn4+Fluorescent ceramic plate
First, K is synthesized2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO2Grinding and mixing the materials in an agate mortar, respectively treating and heating the materials for 30 minutes under flowing HF gas at 300 ℃, and repeating the treatment for 2-3 times. Then hot pressing to prepare ceramic, adding K with different doping concentrations2SiF6:Mn4+The powder is respectively put into a steel die and lined with graphite foil. Then loading the mold into a uniaxial hot press with a vacuum degree of less than 1 × 10 at 500 deg.C-6Pressing under 175MPa in vacuum of Pa, maintaining the pressure for 4 hours, then uniformly releasing the pressure to normal pressure, and finally polishing the surface of the ceramic wafer to obtain the fluorescent ceramic wafer.
Example 5: k2SiF6: 1wt.%Mn4+Fluorescent ceramic plate
First, K is synthesized2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO2Grinding and mixing the materials in an agate mortar, treating and heating the materials for 10 minutes under flowing HF gas at 500 ℃, and repeating the treatment for 2-3 times. Then hot-pressing to prepare ceramic, adding K2SiF6:Mn4+The powder is put into a steel die and lined with graphite foil. Then loading the mold into a uniaxial hot press with a vacuum degree of less than 1 × 10 at 300 deg.C-6Pressing under vacuum of Pa at 150MPa, maintaining the pressure for 2 hours, and then homogenizingThe pressure is released to normal pressure. And finally, polishing the surface of the ceramic wafer to obtain the fluorescent ceramic wafer.
Example 6: k2SiF6:0.1 wt%Mn4+Fluorescent powder
Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, undoped K2SiF6Powder and MnO with mass fraction of 0.1%2Grinding and mixing the materials in an agate mortar, calcining the materials at 500 ℃, and then grinding the materials again to obtain the fluorescent powder.
As can be seen from FIG. 1, the method provided by the present invention successfully synthesizes transparent fluorescent ceramics. Referring to FIG. 2, which shows that the fluorescent ceramic chip exhibits a narrow-band emission in the red region under 450nm excitation, FIG. 3A, B shows the emission spectra of the fluorescent ceramic chip prepared in example 1 and the fluorescent powder prepared in example 6 at 300 degrees Celsius respectively, and it can be seen that K is2SiF6: 0.1 wt%Mn4 +Fluorescent ceramic sheet and K2SiF6:0.1 wt%Mn4+Compared with the fluorescent powder, the thermal stability of the fluorescent powder is obviously improved, and the emission intensity of the fluorescent powder is obviously reduced at 300 ℃.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the above embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the present invention.
Claims (3)
1. The preparation method of the novel red fluorescent ceramic chip is characterized in that the prepared fluorescent ceramic chip meets the components shown in the following formula:
K2SiF6:xMn4+
wherein x is mass fraction, and x is more than 0 and less than or equal to 0.01; the fluorescent ceramic sheet is prepared by adopting a hot pressing method, and the preparation steps are as follows:
step one, synthesizing K2SiF6:Mn4+Weighing commercial K with purity of more than 99.9% according to stoichiometric ratio2SiF6And MnO2As a raw material, the K is2SiF6Powder and MnO2Grinding and mixing the materials in an agate mortar, heating the materials for 10 to 30 minutes under flowing HF gas at the temperature of 300 to 500 ℃, and repeating the steps for 2 to 3 times;
step two, preparing ceramic by hot pressing, and adding K2SiF6:Mn4+Putting the powder into a steel die and lining a graphite foil; then the die is put into a uniaxial hot press, and the vacuum degree is less than 1 multiplied by 10 at 300-500 DEG C-6Pressing under 150-200 MPa in vacuum of Pa, maintaining the pressure for 2-4 hours, then uniformly releasing the pressure to normal pressure, and finally polishing the surface of the ceramic wafer to obtain the fluorescent ceramic wafer.
2. The preparation method of the novel red fluorescent ceramic chip is characterized in that the first step and the second step are carried out in an argon-filled environment.
3. A novel red fluorescent ceramic sheet, characterized in that it is prepared by the preparation method of claim 1 or 2.
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Citations (6)
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CN105950137A (en) * | 2016-05-05 | 2016-09-21 | 中国人民大学 | Mn<4+> doped fluoride red fluorescent powder, preparation method and application thereof |
CN106687562A (en) * | 2014-07-22 | 2017-05-17 | 通用电气公司 | Fluorescent organic light emitting elements having high efficiency |
CN106929015A (en) * | 2015-12-29 | 2017-07-07 | 有研稀土新材料股份有限公司 | Red fluorescence powder, its preparation method and the luminescent device comprising the red fluorescence powder |
CN109097041A (en) * | 2018-08-30 | 2018-12-28 | 合肥工业大学智能制造技术研究院 | Preparation method, product, device and the backlight module of the red fluorescence powder of additive Mn |
CN110423613A (en) * | 2019-07-31 | 2019-11-08 | 中山大学 | A kind of white light LEDs that tetravalence is manganese ion activated large scale emitting red light monocrystal material and preparation method thereof |
US20200303354A1 (en) * | 2019-03-18 | 2020-09-24 | Intematix Corporation | LED Filaments and LED Filament Lamps |
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2020
- 2020-12-14 CN CN202011469879.6A patent/CN112573924A/en not_active Withdrawn
Patent Citations (6)
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CN106687562A (en) * | 2014-07-22 | 2017-05-17 | 通用电气公司 | Fluorescent organic light emitting elements having high efficiency |
CN106929015A (en) * | 2015-12-29 | 2017-07-07 | 有研稀土新材料股份有限公司 | Red fluorescence powder, its preparation method and the luminescent device comprising the red fluorescence powder |
CN105950137A (en) * | 2016-05-05 | 2016-09-21 | 中国人民大学 | Mn<4+> doped fluoride red fluorescent powder, preparation method and application thereof |
CN109097041A (en) * | 2018-08-30 | 2018-12-28 | 合肥工业大学智能制造技术研究院 | Preparation method, product, device and the backlight module of the red fluorescence powder of additive Mn |
US20200303354A1 (en) * | 2019-03-18 | 2020-09-24 | Intematix Corporation | LED Filaments and LED Filament Lamps |
CN110423613A (en) * | 2019-07-31 | 2019-11-08 | 中山大学 | A kind of white light LEDs that tetravalence is manganese ion activated large scale emitting red light monocrystal material and preparation method thereof |
Non-Patent Citations (1)
Title |
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R.A. OSBORNE ET AL.: "New red phosphor ceramic K2SiF6:Mn4+", 《OPTICAL MATERIALS》 * |
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