WO2018058935A1 - 一种发光玻璃陶瓷及其制法与在led照明器件中的应用 - Google Patents
一种发光玻璃陶瓷及其制法与在led照明器件中的应用 Download PDFInfo
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- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000005286 illumination Methods 0.000 title abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 65
- 239000011521 glass Substances 0.000 claims abstract description 49
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 36
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 35
- 238000005498 polishing Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 14
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 230000000630 rising effect Effects 0.000 claims description 8
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 4
- 239000003292 glue Substances 0.000 claims 1
- 230000005284 excitation Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000006064 precursor glass Substances 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 239000005084 Strontium aluminate Substances 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 12
- 239000008393 encapsulating agent Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 238000000295 emission spectrum Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 208000003464 asthenopia Diseases 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000006112 glass ceramic composition Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
- C09K11/773—Chalcogenides with zinc or cadmium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Definitions
- solid-state lighting is widely praised for its low pollution, resource saving and long life, and the most widely used in the market is a white LED packaged by a blue GaN chip and a Ce 3+ :YAG phosphor.
- this type of white LED tends to have a relatively high color temperature (>5000K), which is prone to eye fatigue under long-term illumination and is not conducive to general life lighting.
- the common packaging method in the market is to directly mix the phosphor with the epoxy resin and then apply it on the blue chip. Although this method is simple, the light emitted by the product is prone to chromatic aberration after a period of use.
- the glass ceramic thus formed is not only stable, but also the phosphor is not affected, and has been successfully applied to high-power remote LEDs.
- the packaging material since only the packaging material is changed from epoxy resin to glass ceramic, it cannot change the shortness of light emitted by the package and the high color temperature.
- the primary object of the present invention is to provide an illuminating glass ceramic which has uniform color and good illuminating performance, and can be packaged with an ultraviolet ray chip on the existing market.
- Power remote warm white LEDs enrich existing luminescent materials and make up for the deficiencies of the prior art.
- Another object of the present invention is to provide a method for producing the above-described luminescent glass ceramic.
- Still another object of the present invention is to provide an application of the above-described luminescent glass ceramic in the preparation of an LED lighting device.
- a luminescent glass ceramic composed of a silicate red luminescent glass powder having a mass ratio of 100:0 to 99.1:0.9 and an azure blue phosphor Sr 4 Al 14 O 25 :Eu 2+ .
- silicate red luminescent glass powder is composed of the following mole fraction components:
- a method for preparing the above luminescent glass ceramic comprises the following steps:
- SiO 2 , Na 2 CO 3 , Al 2 O 3 , CaO and Eu 2 O 3 are uniformly mixed, and then placed in a high-temperature box type electric resistance furnace to raise the temperature. After the reaction is completed, the furnace is cooled to room temperature. Grinding the reaction product to obtain a silicate red luminescent glass powder;
- the temperature rising reaction described in the step (1) means that the temperature is raised to 1300 to 1500 ° C at 5 to 10 ° C / min, and then the reaction is kept for 3 to 6 hours.
- the molar ratio of SiO 2 , Na 2 CO 3 , Al 2 O 3 , CaO and Eu 2 O 3 used in the step (1) is (50 to 60): (20 to 30): 9:6:5.
- the mass ratio of the silicate red luminescent glass powder and the Sr 4 Al 14 O 25 :Eu 2+ phosphor used in the step (2) is 100:0 to 99.1:0.9.
- the tableting described in the step (2) means that the tablet is pressed under a pressure of 20 to 40 MPa, preferably at 20 MPa.
- the temperature rising reaction in the step (2) means that the temperature is raised to 650 to 700 ° C at 5 to 10 ° C / min, and the temperature is kept for 0.5 to 10 hours.
- the temperature rising reaction described in the step (2) means raising the temperature to 680 ° C at 5 ° C / min, and maintaining the reaction for 0.5 h.
- the above-mentioned application of the illuminating glass ceramic in the preparation of the LED lighting device comprises the following steps: directly covering the illuminating glass ceramic on the 385 nm ultraviolet illuminating chip, and fixing the illuminating glass ceramic with the high temperature resistant encapsulant, and then obtaining the LED lighting device.
- the mechanism of the invention is:
- the invention obtains an ultraviolet-excited luminescent glass ceramic by mixing azure blue phosphor Sr 4 Al 14 O 25 :Eu 2+ and silicate red luminescent glass powder and sintering at a low temperature. Since the emission wavelength range of the phosphor used is covered at 450 to 550 nm, and the precursor glass powder can simultaneously provide a red light portion, the thus obtained luminescent glass ceramic can obtain warm white light under excitation of a 385 nm ultraviolet chip. By adjusting the ratio of phosphor to glass powder, the types of warm white light are also different, which provides more options for practical applications.
- the present invention has the following advantages and beneficial effects:
- the invention is coated with a luminescent glass ceramic material, which largely isolates the phosphor from contact with the outside to reduce the probability of the phosphor being eroded, and because the luminescent glass ceramic has a high thermal conductivity, it can be very Good application on high power remote LEDs.
- the glass powder used in the present invention is specially designed to emit red light by adding a lanthanum element, and can also emit red light under excitation of a certain wavelength, and is better for low-temperature warm white LED after compounding with the phosphor.
- the application, and adjust the ratio of the two can get warm white LEDs with different color temperatures.
- FIG. 4 is a color coordinate corresponding to the operation of the high-power remote LED obtained by the packages of Embodiments 1 to 6 and the working effect thereof.
- FIG. 5 is a diagram showing color coordinate changes corresponding to the operation of the high-power remote LED in different currents in Embodiment 11.
- FIG. 5 is a diagram showing color coordinate changes corresponding to the operation of the high-power remote LED in different currents in Embodiment 11.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the obtained illuminating glass ceramic is directly covered on the ultraviolet light emitting chip with an emission wavelength of 385 nm, and is fixed at a periphery with a high temperature resistant encapsulant to obtain a high-power remote LED, which is operated at a input current of 90 mA and an input voltage of 16 V for 0.5 h and tested for color of light. performance.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the obtained luminescent glass ceramic is directly covered on an ultraviolet light emitting chip having an emission wavelength of 385 nm.
- a high-power remote LED is obtained by fixing the high-temperature encapsulant at the periphery, and the light color performance is tested by operating at 90 mA input current and 16 V input voltage for 0.5 h.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the mixture is pressed into a sheet under a pressure of 20 MPa, placed in a high temperature box type electric resistance furnace, and heated at 5 ° C / min. After sintering at 680 ° C for 0.5 h, the furnace was cooled to room temperature, and after polishing and polishing, a luminescent glass ceramic was obtained.
- the obtained illuminating glass ceramic is directly covered on the ultraviolet light emitting chip with an emission wavelength of 385 nm, and is fixed at a periphery with a high temperature resistant encapsulant to obtain a high-power remote LED, which is operated at a input current of 90 mA and an input voltage of 16 V for 0.5 h and tested for color of light. performance.
- the excitation and emission spectra of the Sr 4 Al 14 O 25 :Eu 2+ phosphor and the silicate red luminescent glass powder used in Example 4 and the emission spectrum of the prepared luminescent glass ceramic are as shown in FIG. It can be seen in Fig. 1 that the Sr 4 Al1 4 O 25 :Eu 2+ phosphor and the silicate red luminescent glass powder have a common excitation range (for example, 385 nm), and the mixed light of the two can be obtained by excitation at the same wavelength.
- a common excitation range for example, 385 nm
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the obtained illuminating glass ceramic is directly covered on the ultraviolet light emitting chip with an emission wavelength of 385 nm, and is fixed at a periphery with a high temperature resistant encapsulant to obtain a high-power remote LED, which is operated at a input current of 90 mA and an input voltage of 16 V for 0.5 h and tested for color of light. performance.
- the emission spectrum of the luminescent glass ceramics obtained in Examples 1 to 6 is shown in Fig. 2. It can be seen from Fig. 2 that as the phosphor content increases, the emission peak also increases with it, which is beneficial for regulation.
- the luminescent color, the optical performance data of the luminescent glass ceramics obtained in Examples 1 to 6 are shown in Table 1 below:
- the luminescent glass ceramics of Examples 1 to 6 emit light due to the difference in the ratio of the raw materials.
- the color also changes from red to azure blue, and the quantum efficiency at the corresponding wavelength also exhibits regular changes, which can meet the needs of practical applications.
- the emission spectra of the high-power remote LEDs packaged in Examples 1 to 6 are shown in Fig. 3. As can be seen from Fig. 3, the obtained LED emission spectrum can correspond well to the emission spectrum of the glass ceramic.
- the color coordinates corresponding to the high-power remote LEDs packaged in the embodiments 1 to 6 and the working effect diagrams thereof are shown in Fig. 4. As can be seen from Fig. 4, as the phosphor content increases, it can be obtained. Different kinds of warm white LEDs.
- optical performance data of the high-power remote LEDs packaged in Examples 1 to 6 are shown in Table 2 below:
- each raw material in the silicate red luminescent glass powder 50% SiO 2 , 30% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the mixture is pressed into a sheet under a pressure of 20 MPa, placed in a high temperature box type electric resistance furnace, and heated at 5 ° C / min. After sintering at 680 ° C for 0.5 h, the furnace was cooled to room temperature, and after polishing and polishing, a luminescent glass ceramic was obtained.
- the obtained luminescent glass ceramic is directly covered on the ultraviolet ray emitting chip with an emission wavelength of 385 nm, and is fixed at a periphery by using a high temperature resistant encapsulant to obtain a high-power remote LED, which is input at 90 mA.
- the current and the 16V input voltage were operated for 0.5h and tested for light color performance.
- each raw material in the silicate red luminescent glass powder 50% SiO 2 , 30% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is thoroughly mixed, placed in a high temperature box type electric resistance furnace, and heated to 1500 ° C at 10 ° C / min. After 5 h of heat preservation, the furnace is cooled to room temperature and then ground to obtain a silicate red luminescent glass powder.
- the mixture is pressed into a sheet under a pressure of 20 MPa, placed in a high temperature box type electric resistance furnace, and heated at 5 ° C / min. After sintering at 680 ° C for 0.5 h, the furnace was cooled to room temperature, and after polishing and polishing, a luminescent glass ceramic was obtained.
- the obtained illuminating glass ceramic is directly covered on the ultraviolet light emitting chip with an emission wavelength of 385 nm, and is fixed at a periphery with a high temperature resistant encapsulant to obtain a high-power remote LED, which is operated at a input current of 90 mA and an input voltage of 16 V for 0.5 h and tested for color of light. performance.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the mixture is fully mixed, pressed at 40MPa pressure to form a sheet, placed in a high temperature box type resistance furnace, heated at 10 ° C / min After sintering at 650 ° C for 0.5 h, the furnace was cooled to room temperature, and after polishing and polishing, a luminescent glass ceramic was obtained.
- each raw material in the silicate red luminescent glass powder 60% SiO 2 , 20% Na 2 CO 3 , 9% Al 2 O 3 , 6% CaO, 5% Eu 2 O 3 ratio is fully mixed, placed in a high temperature box type resistance furnace, heated to 1300 ° C at 5 ° C / min, after 3 h of heat preservation, after cooling to room temperature with the furnace, grinding, to obtain silicate red luminescent glass powder.
- the mixture is fully mixed, pressed at 40MPa pressure to form a sheet, placed in a high temperature box type resistance furnace, heated at 10 ° C / min After sintering at 700 ° C for 1 h, the furnace was cooled to room temperature, and after polishing and polishing, a luminescent glass ceramic was obtained.
- the obtained illuminating glass ceramic is directly covered on the ultraviolet light emitting chip with an emission wavelength of 385 nm, and is fixed at a periphery with a high temperature resistant encapsulant to obtain a high-power remote LED, which is operated at a input current of 90 mA and an input voltage of 16 V for 0.5 h and tested for color of light. performance.
- the luminescent glass ceramic obtained in Example 4 of the present invention and the ultraviolet ray emitting chip having an emission wavelength of 385 nm were packaged into a high-power remote LED, and operated at 20 to 90 mA input current and 16 V input voltage for 0.5 h and tested for light color performance.
- the color coordinate change diagram corresponding to the operation of the high-power remote LED at different currents is shown in Fig. 5. It can be seen from Fig. 5 that the color of the LED light obtained changes with the change of the current, but in the Acceptable range.
- optical performance data of the high power remote LEDs packaged in Example 11 are shown in Table 3 below:
- Example 4 luminescent glass ceramic 20 0.3708 0.4107 UV chip + Example 4 luminescent glass ceramic 30 0.3706 0.4075 UV chip + Example 4 luminescent glass ceramic 40 0.3705 0.4041 UV chip + Example 4 luminescent glass ceramic 50 0.371 0.4008 UV chip + Example 4 luminescent glass ceramic 60 0.3715 0.3972 UV chip + Example 4 luminescent glass ceramic 70 0.3726 0.3935 UV chip + Example 4 luminescent glass ceramic 80 0.3739 0.3896 UV chip + Example 4 luminescent glass ceramic 90 0.3756 0.3855
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Abstract
Description
组成 | 色坐标X | 色坐标Y | 色温 |
紫外芯片+实施例1发光玻璃陶瓷 | 0.5651 | 0.2624 | 56930 |
紫外芯片+实施例2发光玻璃陶瓷 | 0.5024 | 0.3061 | 3116 |
紫外芯片+实施例3发光玻璃陶瓷 | 0.4301 | 0.3508 | 2496 |
紫外芯片+实施例4发光玻璃陶瓷 | 0.3706 | 0.3861 | 4320 |
紫外芯片+实施例5发光玻璃陶瓷 | 0.3575 | 0.3961 | 4752 |
紫外芯片+实施例6发光玻璃陶瓷 | 0.3329 | 0.4131 | 5531 |
组成 | 输入电流 | 色坐标X | 色坐标Y |
紫外芯片+实施例4发光玻璃陶瓷 | 20 | 0.3708 | 0.4107 |
紫外芯片+实施例4发光玻璃陶瓷 | 30 | 0.3706 | 0.4075 |
紫外芯片+实施例4发光玻璃陶瓷 | 40 | 0.3705 | 0.4041 |
紫外芯片+实施例4发光玻璃陶瓷 | 50 | 0.371 | 0.4008 |
紫外芯片+实施例4发光玻璃陶瓷 | 60 | 0.3715 | 0.3972 |
紫外芯片+实施例4发光玻璃陶瓷 | 70 | 0.3726 | 0.3935 |
紫外芯片+实施例4发光玻璃陶瓷 | 80 | 0.3739 | 0.3896 |
紫外芯片+实施例4发光玻璃陶瓷 | 90 | 0.3756 | 0.3855 |
Claims (7)
- 一种发光玻璃陶瓷,其特征在于由质量比为100:0~99.1:0.9的硅酸盐红色发光玻璃粉和天青蓝色荧光粉Sr4Al14O25:Eu2+构成。
- 一种根据权利要求1或2所述的发光玻璃陶瓷的制备方法,其特征在于包括以下步骤:(1)将SiO2、Na2CO3、Al2O3、CaO和Eu2O3混合均匀,然后置于高温箱式电阻炉中,升温反应,待反应完成后随炉冷却至室温后,将反应产物研磨即得到硅酸盐红色发光玻璃粉;(2将步骤(1)中得到的硅酸盐红色发光玻璃粉和Sr4Al14O25:Eu2+荧光粉混合均匀,然后将其压片并置于高温箱式电阻炉中,升温反应,反应结束后随炉冷却至室温,经过打磨、抛光后得到发光玻璃陶瓷。
- 根据权利要求3所述的发光玻璃陶瓷的制备方法,其特征在于:步骤(1)中所述的升温反应是指以5~10℃/min升温至1300~1500℃,然后保温反应3~6h;步骤(2)中所述的升温反应是指以5~10℃/min升温至650~700℃,保温反应0.5~1h;步骤(2)中所述的压片是指在20~40MPa压力下压制成片。
- 根据权利要求3所述的发光玻璃陶瓷的制备方法,其特征在于:步骤(1)中所述的升温反应是指以5℃/min升温至1300℃,然后保温反应3h;步骤(2)中所述的升温反应是指以5℃/min升温至680℃,保温反应0.5h;步骤(2)中所述的压片是指在20MPa压力下压制成片。
- 根据权利要求3所述的发光玻璃陶瓷的制备方法,其特征在于:步骤(1)中所使用的SiO2、Na2CO3、Al2O3、CaO和Eu2O3的摩尔比为(50~60):(20~30):9:6:5;步骤(2)中所使用的硅酸盐红色发光玻璃粉和Sr4Al14O25:Eu2+荧光粉的质量比为100:0~99.1:0.9。
- 根据权利要求1或2所述的发光玻璃陶瓷在制备LED照明器件中的应用,具体包括以下步骤:在385nm紫外发光芯片上直接覆盖权利要求1或2所述的发光玻璃陶瓷,使用耐高温封装胶于周边进行固定后即得到LED照明器件。
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CN113372911A (zh) * | 2021-05-27 | 2021-09-10 | 华北电力大学科技学院 | 一种氧化铝基体的红色荧光粉及其制备方法 |
CN114479859A (zh) * | 2022-01-05 | 2022-05-13 | 浙江大学 | 一种多色可调锗酸盐荧光玻璃陶瓷及其制备方法 |
CN115893847A (zh) * | 2022-10-25 | 2023-04-04 | 福建江夏学院 | 一种多模荧光微晶玻璃及其制备与应用 |
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