CN113004891A - Fluorescent powder and LED light source - Google Patents
Fluorescent powder and LED light source Download PDFInfo
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- CN113004891A CN113004891A CN202110142062.6A CN202110142062A CN113004891A CN 113004891 A CN113004891 A CN 113004891A CN 202110142062 A CN202110142062 A CN 202110142062A CN 113004891 A CN113004891 A CN 113004891A
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- 239000000843 powder Substances 0.000 title claims abstract description 66
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 109
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 108
- 239000000203 mixture Substances 0.000 claims abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 29
- 230000005284 excitation Effects 0.000 claims description 19
- 239000003292 glue Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 6
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 239000008393 encapsulating agent Substances 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 18
- 238000001228 spectrum Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 12
- 230000000295 complement effect Effects 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 24
- 238000002156 mixing Methods 0.000 description 13
- 229910001868 water Inorganic materials 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 9
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 8
- 238000000295 emission spectrum Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002189 fluorescence spectrum Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910021617 Indium monochloride Inorganic materials 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
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- 239000000084 colloidal system Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 238000000695 excitation spectrum Methods 0.000 description 1
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- 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
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/75—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth containing antimony
- C09K11/755—Halogenides
- C09K11/756—Halogenides with alkali or alkaline earth metals
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- 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
- H01L33/504—Elements with two or more wavelength conversion materials
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- 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
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- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention belongs to the technical field of luminescent materials, and particularly relates to fluorescent powder and an LED light source. The fluorescent powder provided by the invention comprises antimony doped Cs2NaInCl6And antimony doped Cs2InCl5·H2And the mixture of O and the two materials with the same luminescent mechanism is mixed, so that under the condition that the self-trapping excitons of the two materials emit light with different self-trapping excitons, the complementary effect of the luminescent ranges is realized, the wide-spectrum light emission effect from blue light to yellow light can be realized, and the fluorescent quantum efficiency is as high as 73 percent. The fluorescent powder is used in an LED light source, can enable the LED light source to realize various light-emitting effects, and has good light-emitting performance.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to fluorescent powder and an LED light source.
Background
The Light Emitting Diode (LED) has the advantages of high luminous efficiency, low energy consumption, long service life, no pollution and the like, and is widely applied to the fields of illumination and display. In the light realization process of the LED, the performance indexes of the LED such as luminous efficiency, color temperature and the like are determined by the selection of the fluorescent powder. The conventional fluorescent powder has the problems of narrow emission peak and low quantum yield, so that the luminous performance of the LED is limited.
Therefore, how to obtain the phosphor emitting light with wide spectrum and improve the quantum yield of the phosphor is one of the current research directions of the LED.
Disclosure of Invention
The invention aims to provide fluorescent powder and an LED light source, and aims to solve the technical problems of narrow emission peak, low quantum yield and the like of the conventional fluorescent powder.
In order to achieve the above objects, according to one aspect of the present invention, there is provided a phosphor including antimony-doped Cs2NaInCl6(Cs2NaInCl6Sb) and Sb-doped Cs2InCl5·H2O(Cs2InCl5·H2O: Sb) are used.
Antimony doped Cs2NaInCl6Can emit wide-spectrum blue light under the excitation of ultraviolet light, and is doped with antimony and Cs2InCl5·H2O can emit yellow light with broad spectrum under the excitation of ultraviolet light, and both are doped with antimony (Sb)3+) As a luminescence center, by s2The → sp transition achieves fluorescence emission. However, these two materials are different in crystal structure, Sb3+The difference of lattice environment causes the difference of self-trapped excitons (STEs) to emit light. According to the invention, the two materials with the same luminescence mechanism are mixed, so that under the condition that the self-trapping excitons of the two materials emit light with different self-trapping excitons, the complementary effect of the luminescence range is realized, the wide-spectrum light emission effect from blue light to yellow light can be realized, and the fluorescence quantum efficiency is as high as 73%. Meanwhile, the fluorescent powder provided by the invention is prepared by adjusting the antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O can realize various light-emitting effects including warm white light, cold white light and the like, and is an ideal lighting material.
As a preferred technical scheme of the fluorescent powder, the antimony is doped with Cs2NaInCl6With said antimony doped Cs2InCl5·H2The molar ratio of O is (1-9) to (1-9).
As a preferred technical scheme of the fluorescent powder, the antimony is doped with Cs2NaInCl6In the step (b), the doping amount of the antimony is 1-10%.
As a preferred technical scheme of the fluorescent powder, the antimony is doped with Cs2InCl5·H2In O, the doping amount of the antimony is 1% -10%.
As a preferable technical scheme of the fluorescent powder, the light-emitting color coordinate range of the fluorescent powder is (0.17, 0.13) - (0.50, 0.40).
As a preferable technical scheme of the fluorescent powder, the excitation wavelength of the fluorescent powder is 300nm-350 nm.
In another aspect of the invention, an LED light source is provided, which includes a chip and a fluorescent glue encapsulated on the chip, wherein the fluorescent glue includes an encapsulating glue and a fluorescent powder for exciting the chip to generate emission waves; wherein the fluorescent powder is the fluorescent powder provided by the invention.
The LED light source provided by the invention has the advantages that the used fluorescent powder realizes the wide-spectrum light emission effect from blue light to yellow light, and the fluorescence quantum efficiency is up to 73%, so the LED light source has higher luminous efficiency and wider luminous spectrum. By adjusting the antimony doped Cs in the fluorescent powder2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O can enable the LED light source provided by the invention to realize various light-emitting effects, and the LED light source has a good application prospect.
As a preferred technical scheme of the LED light source, in the fluorescent powder, the antimony is doped with Cs2NaInCl6With said antimony doped Cs2InCl5·H2When the molar ratio of O is (4-5) to (5-6), the LED light source is a white light source.
As a preferable technical scheme of the LED light source, the particle size of the fluorescent powder is 1-100 μm.
As a preferable technical scheme of the LED light source, the chip is an ultraviolet chip.
As a preferable technical scheme of the LED light source, the emission wavelength of the chip is 300nm-350 nm.
As a preferred technical scheme of the LED light source, the packaging adhesive is ultraviolet-resistant silica gel.
Drawings
FIG. 1 shows Sb-doped Cs2NaInCl6And antimony doped Cs2InCl5·H2Excitation and emission spectra of O;
FIG. 2 shows Sb-doped Cs2NaInCl6A plot of fluorescence quantum efficiency under 320nm excitation light;
FIG. 3 shows Sb-doped Cs2InCl5·H2A plot of fluorescence quantum efficiency of O under 310nm excitation light;
FIG. 4 is a graph of fluorescence quantum efficiency of the phosphor provided in example 2 of the present invention under 310nm excitation light;
FIG. 5 is a color coordinate and color temperature chart corresponding to the fluorescence spectrum of the phosphor provided in embodiments 1-4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and technical effects of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and the embodiments described below are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention. Those whose specific conditions are not specified in the examples are carried out according to conventional conditions or conditions recommended by the manufacturer; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, the term "and/or" describing an association relationship of associated objects means that there may be three relationships, for example, a and/or B, may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the description of the present invention, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a. b, c, a-b (i.e. a and b), a-c, b-c, or a-b-c, wherein a, b, and c can be single or multiple respectively.
It should be understood that the weight of the related components mentioned in the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, it is within the scope of the disclosure that the content of the related components is scaled up or down according to the embodiments of the present invention. Specifically, the weight described in the embodiments of the present invention may be a unit of mass known in the chemical field such as μ g, mg, g, kg, etc.
In addition, unless the context clearly uses otherwise, an expression of a word in the singular is to be understood as including the plural of the word. The terms "comprises" or "comprising" are intended to specify the presence of stated features, quantities, steps, operations, elements, portions, or combinations thereof, but are not intended to preclude the presence or addition of one or more other features, quantities, steps, operations, elements, portions, or combinations thereof.
The embodiment of the invention provides fluorescent powder which comprises antimony doped Cs2NaInCl6(Cs2NaInCl6Sb) and Sb-doped Cs2InCl5·H2O(Cs2InCl5·H2O: Sb) are used.
The embodiment of the invention dopes antimony with Cs by the same luminous mechanism2NaInCl6And antimony doped Cs2InCl5·H2And O is mixed, so that under the condition that the self-trapping excitons and the self-trapping excitons emit light with different ranges, the complementary effect of the light emitting ranges is realized, the wide-spectrum light emitting effect from blue light to yellow light can be realized, and the fluorescence quantum efficiency is as high as 73 percent. Meanwhile, the fluorescent powder provided by the embodiment of the invention adjusts the antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O can realize various light-emitting effects including warm white light, cold white light and the like, and is an ideal lighting material.
Antimony doped Cs2NaInCl6And the broad-spectrum blue light emission (the peak wavelength is 450nm) can be realized under the excitation of 320nm ultraviolet light. Antimony doped Cs2InCl5·H2O, and can emit broad-spectrum yellow light under the excitation of ultraviolet light at 310nm (the peak wavelength is 610 nm). As shown in FIG. 1, it can be seen that antimony is doped with Cs2NaInCl6The excitation wavelength of the light source is 310nm-340nm, and the emission wavelength of the light source is 400nm-550 nm; antimony doped Cs2InCl5·H2The excitation wavelength of O is 300nm-350nm, and the emission wavelength is 450nm-800 nm. Thus, antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2O has a similar excitation range and, in some embodiments, contains antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2The excitation wavelength of the fluorescent powder of O is 300nm-350 nm.
In some embodiments, antimony is doped with Cs2NaInCl6In the above-mentioned step (b), the doping amount of antimony is 1% -10%, preferably 1%. Specifically, typical but non-limiting amounts of doping are 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%. By adjusting the antimony doped Cs2NaInCl6The doping amount of the antimony can be changed to change the antimony doping Cs2NaInCl6The luminous intensity and the fluorescence quantum efficiency of (c). The inventor of the invention found in research that when the doping amount of antimony is 1%, the antimony is doped with Cs2NaInCl6The fluorescence quantum efficiency of (2) is as high as 85%, and the excitation wavelength is 310nm-340nm, as shown in figure 2. As can be seen from FIG. 2, when the doping amount of antimony is 1%, the antimony is doped with Cs2NaInCl6The fluorescence quantum efficiency under excitation light of 320nm was 85.47%, and the peak wavelength thereof was 450 nm.
In some embodiments, antimony is doped with Cs2InCl5·H2In O, the doping amount of antimony is 1-10%, preferably 1%. Specifically, typical but non-limiting amounts of doping are 1%, 2%, 3%, 4%,5%, 6%, 7%, 8%, 9%, 10%. By adjusting the antimony doped Cs2InCl5·H2The doping amount of antimony in O can be changed to dope Cs with antimony2InCl5·H2The luminous intensity of O and the fluorescence quantum efficiency. The inventor of the invention found in research that when the doping amount of antimony is 1%, the antimony is doped with Cs2InCl5·H2The fluorescence quantum efficiency of O is as high as 88%, and the excitation wavelength is 300nm-350nm, as shown in FIG. 3. As can be seen from FIG. 3, when the doping amount of antimony is 1%, the antimony is doped with Cs2InCl5·H2The fluorescence quantum efficiency of O under the excitation light of 310nm is 88.09%.
Antimony doped Cs2NaInCl6And antimony doped Cs2InCl5·H2O has the same mechanism of light emission, both with doped antimony (Sb)3+) As a luminescence center, by s2The → sp transition achieves fluorescence emission. However, these two materials are different in crystal structure, Sb3+The difference of lattice environment causes the difference of self-trapped excitons (STEs) to emit light. The invention mixes the two materials, thereby realizing the complementation of the light emitting range under the condition that the self-trapping excitons and the self-trapping excitons emit light with a difference, and obtaining the wide-spectrum light emitting effect from blue light to yellow light. In some embodiments, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O is (3-6) to (4-7). By adjusting the molar ratio between the fluorescent powder and the fluorescent powder, the obtained fluorescent powder has various spectral characteristics, and realizes various luminous effects so as to be applied to illumination of different occasions. Specifically, antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2Typical but non-limiting molar ratios between O are 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 2:1, 2:3, 2:5, 2:7, 2:9, 3:1, 3:2, 3:4, 3:5, 3:7, 3:8, 4:1, 4:3, 4:5, 4:7, 4:9, 5:1, 5:2, 5:3, 5:4, 5:6, 5:7, 5:8, 5:9, 6:1, 6:5, 6:7, 7:1, 7:2, 7:3, 7:4, 7:5, 7:6, 7:8, 7:9, 8:1, 8:3, 8:5, 8:7, 8:9, 9:1, 9:2, 9:4, 9:5, 9: 9, 9: 5: 6.
The inventionThe phosphor provided in the examples had a light emission color coordinate ranging from (0.17, 0.13) to (0.50, 0.40). Namely by adjusting the antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O, the obtained fluorescent powder can realize all the luminous effects in the color coordinate range.
In one embodiment, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When the molar ratio of O is 3:7, the color coordinate corresponding to the fluorescent spectrum of the obtained fluorescent powder is CIE (0.43, 0.38).
In another embodiment, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When the molar ratio of O is 4:6, the color coordinate corresponding to the fluorescent spectrum of the obtained fluorescent powder is CIE (0.37, 0.33), and the fluorescent powder belongs to warm white light.
In yet another embodiment, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When the molar ratio of O is 5:5 (namely 1:1), the color coordinate corresponding to the fluorescence spectrum of the obtained fluorescent powder is CIE (0.32, 0.27), and the fluorescent powder belongs to cold white light.
In yet another embodiment, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When the molar ratio of O is 6:4 (i.e. 3:2), the color coordinate corresponding to the fluorescence spectrum of the obtained phosphor is CIE (0.26, 0.21).
The fluorescent powder provided by the embodiment of the invention can be prepared by the following method.
The embodiment of the invention provides a preparation method of fluorescent powder, which comprises the step of doping antimony with Cs2NaInCl6With antimony doped Cs2InCl5·H2And mixing and processing O according to a molar ratio to obtain the fluorescent powder.
The preparation method of the fluorescent powder provided by the embodiment of the invention only needs to dope antimony with Cs2NaInCl6With antimony doped Cs2InCl5·H2The phosphor powder can be obtained by mixing O, and has the advantages of simple operation and easy implementationThe production efficiency of the fluorescent powder is improved.
In the fluorescent powder provided by the embodiment of the invention, antimony is doped with Cs2NaInCl6The preparation method can be adopted to prepare the following components:
s11, providing a first solution containing NaCl and a second solution containing CsCl;
s12, providing a solution containing InCl3And SbCl3And adjusting the pH of the solution to be less than 4.0;
s13, mixing the first solution, the second solution and the third solution for reaction to obtain a mixed solution, and separating and purifying the mixed solution to obtain the antimony-doped Cs2NaInCl6。
In S11, the first solution containing NaCl preferably has a molar concentration of 6 mol/L; the molar concentration of the second solution containing CsCl was 4 mol/L.
In S12, 2mmol of InCl is preferably added3And 0.02mmol of SbCl3Dissolved in 1mL of ultrapure water, and adjusted dropwise with 50. mu.L of concentrated hydrochloric acid to obtain a third solution.
In S13, the second solution and the third solution are preferably mixed in a ratio of 1:1, carrying out centrifugal separation after full reaction, washing twice with isopropanol, and drying at 60 ℃ to obtain the antimony-doped Cs2NaInCl6。
In the fluorescent powder provided by the embodiment of the invention, antimony is doped with Cs2InCl5·H2The preparation method of O can be prepared by adopting the following steps:
s21, providing a first solution containing CsCl;
s22, providing a solution containing InCl3And SbCl3And adjusting the pH of the solution to be less than 4.0;
s23, mixing the first solution and the second solution for reaction to obtain a mixed solution, and separating and purifying the mixed solution to obtain antimony-doped Cs2InCl5·H2O。
In S21, the CsCl-containing first solution preferably has a molar concentration of 4 mol/L.
In S22, 2mmol of InCl is preferably added3And 0.02mmol of SbCl3Dissolved in 1mL of ultrapure water, and adjusted dropwise with 50. mu.L of concentrated hydrochloric acid to obtain a second solution.
In S23, the first solution and the second solution are preferably mixed in a ratio of 1:1, performing centrifugal separation after full reaction, washing twice with isopropanol, and drying at 60 ℃ to obtain antimony-doped Cs2InCl5·H2O。
In the preparation method of the fluorescent powder provided by the embodiment of the invention, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2The selection, doping amount, and molar ratio of the two and the light emitting effect of O are as described above, and are not described herein again. The embodiment of the invention dopes the antimony with the Cs2NaInCl6With antimony doped Cs2InCl5·H2The method for mixing treatment of O can adopt the conventional method in the field, including but not limited to mixing grinding, ultrasonic mixing, stirring and mixing and the like.
In some embodiments, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When O is mixed according to the mol ratio, selecting the antimony doped Cs with the average grain diameter of 1-100 mu m2NaInCl6And antimony-doped Cs with average particle size of 1-100 μm2InCl5·H2And O. By selecting antimony doped Cs with smaller particle size2NaInCl6And antimony doped Cs2InCl5·H2And O, the mixing effect of the fluorescent powder and the organic light-emitting material can be more sufficient, so that the uniformity of the obtained fluorescent powder is improved, and the light-emitting performance and the lighting effect of the fluorescent powder are improved. Specifically, antimony doped Cs2NaInCl6Typical but not limiting average particle sizes are 1 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm; antimony doped Cs2InCl5·H2O typically has a non-limiting average particle size of 1 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm.
The embodiment of the invention also provides an LED light source which comprises a chip and the fluorescent glue packaged on the chip, wherein the fluorescent glue comprises packaging glue and fluorescent powder for exciting the chip to generate emission waves; the fluorescent powder is provided by the embodiment of the invention.
According to the LED light source provided by the embodiment of the invention, the used fluorescent powder realizes a wide-spectrum light emission effect from blue light to yellow light, and the fluorescence quantum efficiency is up to 73%, so that the LED light source has higher luminous efficiency and wider luminous spectrum. By adjusting the antimony doped Cs in the fluorescent powder2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O can enable the LED light source provided by the embodiment of the invention to realize various light-emitting effects, and the LED light source has a good application prospect.
White light LED light sources are the most widely used light sources with the greatest practical requirements. In some embodiments, the Cs is doped by adjusting the antimony in the phosphor2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O is (4-5) to (5-6), so that the obtained LED light source can realize white light emission. Further, by adjusting the antimony doped Cs in the fluorescent powder2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O can also enable the obtained LED light source to realize warm white light emission or cold white light emission of nearly pure white light. In one embodiment, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When the molar ratio of O is 4:6, the obtained LED light source emits warm white light. In another embodiment, antimony is doped with Cs2NaInCl6With antimony doped Cs2InCl5·H2When the molar ratio of O is 5:5 (i.e., 1:1), the resulting LED light source emits cool white light.
In some embodiments, the uv chip is selected to excite the phosphor to produce emission waves. Specifically, the excitation wavelength of the phosphor provided by the embodiment of the invention is 300nm to 350nm, so that a chip with an emission wavelength of 300nm to 350nm is preferable.
In some embodiments, the encapsulant is an ultraviolet resistant silicone. The anti-ultraviolet silica gel is selected, cannot be influenced by ultraviolet rays, has the advantages of low stress and low possibility of damage, has excellent refractive index and light transmittance, can ensure that the colloid and the fluorescent powder are mixed and then reduce or avoid influencing the brightness of an LED light source as far as possible, ensures the output of luminous flux to the maximum extent, and avoids the occurrence of color temperature drift phenomenon.
In order to make the above implementation details and operations of the present invention clearly understood by those skilled in the art and to make the advanced performance of the phosphor and the LED light source of the embodiments of the present invention obviously manifest, the above technical solutions are illustrated by the following embodiments.
Example 1
The embodiment provides a fluorescent powder, and a preparation method thereof is as follows:
doping antimony with Cs2NaInCl6(doping amount is 1%) and antimony-doped Cs2InCl5·H2And mixing and grinding O (the doping amount is 1%) according to a molar ratio of 3:7 to obtain the fluorescent powder.
Example 2
The embodiment provides a fluorescent powder, and a preparation method thereof is as follows:
doping antimony with Cs2NaInCl6(doping amount is 1%) and antimony-doped Cs2InCl5·H2And mixing O (the doping amount is 1%) according to a molar ratio of 4:6 to obtain the fluorescent powder.
Example 3
The embodiment provides a fluorescent powder, and a preparation method thereof is as follows:
doping antimony with Cs2NaInCl6(doping amount is 1%) and antimony-doped Cs2InCl5·H2And mixing O (the doping amount is 1%) according to a molar ratio of 5:5 to obtain the fluorescent powder.
Example 4
The embodiment provides a fluorescent powder, and a preparation method thereof is as follows:
doping antimony with Cs2NaInCl6(doping amount is 1%) and antimony-doped Cs2InCl5·H2Mixing O (the doping amount is 1%) according to a molar ratio of 6:4 to obtain the fluorescent powder。
Experimental example 1
The fluorescence quantum efficiency of the phosphor obtained in example 2 was measured, and the results are shown in fig. 4. As can be seen from FIG. 4, the fluorescence quantum efficiency is 73.20% under the excitation of ultraviolet light at 310 nm.
Experimental example 2
The fluorescence spectra of the phosphors obtained in examples 1 to 4 were measured, and the corresponding color coordinates and color temperature maps are shown in FIG. 5. The spectrally corresponding fluorescence color can be visually reflected by fig. 5. The color coordinate corresponding to the emission spectrum of the phosphor obtained in example 1 is CIE (0.43, 0.38), and yellow light emission can be realized; the color coordinate corresponding to the emission spectrum of the phosphor obtained in example 2 is CIE (0.37, 0.33), and warm white light emission can be realized; the color coordinate corresponding to the emission spectrum of the phosphor obtained in example 3 is CIE (0.32, 0.27), and the emission of cold white light can be realized; the emission spectrum of the phosphor obtained in example 4 has CIE (0.26, 0.21) coordinates, and blue light emission can be realized. Therefore, the fluorescent powder provided by the embodiment of the invention adjusts the antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2The molar ratio of O can realize the wide-spectrum luminous emission effect from blue light to yellow light.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The fluorescent powder is characterized by comprising antimony doped Cs2NaInCl6With antimony doped Cs2InCl5·H2A mixture of O.
2. The phosphor of claim 1, wherein said phosphor is selected from the group consisting ofThen, the antimony is doped with Cs2NaInCl6With said antimony doped Cs2InCl5·H2The molar ratio of O is (1-9) to (1-9).
3. The phosphor of claim 1, wherein the phosphor has a light emission color coordinate ranging from (0.17, 0.13) - (0.50, 0.40).
4. The phosphor of claim 1, wherein said antimony doped Cs2NaInCl6In the step (b), the doping amount of the antimony is 1-10%.
5. The phosphor of claim 1, wherein said antimony doped Cs2InCl5·H2In O, the doping amount of the antimony is 1% -10%.
6. The phosphor of any of claims 1-5, wherein the excitation wavelength of the phosphor is from 300nm to 350 nm.
7. An LED light source is characterized by comprising a chip and fluorescent glue packaged on the chip, wherein the fluorescent glue comprises packaging glue and fluorescent powder for exciting the chip to generate emission waves; wherein the phosphor is the phosphor according to any one of claims 1 to 6.
8. The LED light source of claim 7 wherein the phosphor is characterized by the antimony doped Cs2NaInCl6With said antimony doped Cs2InCl5·H2When the molar ratio of O is (4-5) to (5-6), the LED light source is a white light source.
9. The LED light source of claim 7 wherein the phosphor has an average particle size of 1-100 μ ι η; and/or
The chip is an ultraviolet chip; and/or
The emission wavelength of the chip is 300nm-350 nm.
10. The LED light source of any of claims 7-9, wherein the encapsulant is uv-resistant silicone.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102229802A (en) * | 2011-04-14 | 2011-11-02 | 东北师范大学 | Rare earth double primary colour luminescent material for converting white light by utilizing violet light LED (light-emitting diode) and preparation method thereof |
CN111205861A (en) * | 2020-01-13 | 2020-05-29 | 广西大学 | Sb-doped Cs2AInCl6Double perovskite material and preparation method and application thereof |
-
2021
- 2021-02-02 CN CN202110142062.6A patent/CN113004891A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102229802A (en) * | 2011-04-14 | 2011-11-02 | 东北师范大学 | Rare earth double primary colour luminescent material for converting white light by utilizing violet light LED (light-emitting diode) and preparation method thereof |
CN111205861A (en) * | 2020-01-13 | 2020-05-29 | 广西大学 | Sb-doped Cs2AInCl6Double perovskite material and preparation method and application thereof |
Non-Patent Citations (5)
Title |
---|
AGNIESZKA NOCULAK ET AL.,: ""Bright Blue and Green Luminescence of Sb(III) in Double Perovskite Cs2MInCl6 (M = Na, K) Matrices"", 《CHEM. MATER.》 * |
YUYU JING ET AL.,: ""Sb3+ Dopant and Halogen Substitution Triggered Highly Efficient and Tunable Emission in Lead-Free Metal Halide Single Crystals"", 《CHEM. MATER.》 * |
李宏 等: "《新型特种玻璃》", 31 January 2020, 武汉理工大学出版社 * |
胡庆生 等: "《现代电气工程使用技术手册》", 30 October 1994, 机械工业出版社 * |
马鹏起 等: "《中国稀土强国之梦》", 30 October 2017, 冶金工业出版社 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115725294A (en) * | 2022-11-02 | 2023-03-03 | 北京科技大学 | 0D antimony-doped indium-based inorganic luminescent material and preparation method and application thereof |
CN115725294B (en) * | 2022-11-02 | 2023-09-22 | 北京科技大学 | 0D antimony doped indium-based inorganic luminescent material and preparation method and application thereof |
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