CN114933900B - Ultra-wideband green light emitting phosphate fluorescent material and preparation method thereof - Google Patents
Ultra-wideband green light emitting phosphate fluorescent material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 18
- 239000010452 phosphate Substances 0.000 title claims abstract description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 150000003839 salts Chemical class 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 8
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 abstract description 8
- 238000006862 quantum yield reaction Methods 0.000 abstract description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 6
- 238000006467 substitution reaction Methods 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 230000000875 corresponding effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000009877 rendering Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002060 circadian Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- 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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7795—Phosphates
- C09K11/7796—Phosphates with alkaline earth metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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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Abstract
The invention relates to an ultra-wideband green light emission phosphate fluorescent material and a preparation method thereof. The invention selects K 3 La(PO 4 ) 2 As a base material, eu 2+ The ultra-wideband green light emitting luminescent material is prepared by adopting a traditional high-temperature solid phase method for activating ions and is used for eliminating the green light gap phenomenon. In the preparation of K 3 La(PO 4 ) 2 :Eu 2+ In the luminescent material, a bivalence substitution strategy is utilized to improve the quantum yield and enhance the emission intensity and the thermal stability. The product of the invention is synthesized by a high-temperature solid phase method, and the prepared product has good grain growth quality, few surface defects, loose product, easy crushing, easy scale enlargement and mass production and no influence on the luminescence property.
Description
Technical Field
The invention belongs to the technical field of fluorescent materials, and particularly relates to an ultra-wideband green light emitting phosphate fluorescent material and a preparation method thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Currently, the mainstream commercial phosphor-converted white light emitting diode (pc-WLED) is based on a blue LED chip and Y 3 Al 5 O 12 :Ce 3+ (YAG:Ce 3+ ) And (3) combination of yellow fluorescent powder. Such WLEDs have a low color rendering index (Ra) due to the absence of the red component<80 High color temperature (CCT)>6000K) The above-mentioned disadvantages. Although by adding red CaAlSiN additionally 3 :Eu 2+ The phosphor can improve the color rendering index Ra and the correlated color temperature CCT, but the WLED prepared by this method cannot completely cover the cyan region (480-520 nm) between blue and green light, which results in the color rendering index being usually less than 95, which is the so-called "green gap" phenomenon. In addition, the strong unconverted blue light emitted by the LED chip can have deleterious effects on our health, including contributing to our circadian rhythmNegative effects. Therefore, the development of "adapted" phosphors with high quantum efficiency and emission intensity, excellent thermal stability and tunable emission color is of great significance for full-spectrum WLED illumination.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an ultra-wideband green light emission phosphate fluorescent material and a preparation method thereof, and provides a new alkaline site double aliovalent substitution design method. The preparation method of the ultra-wideband green luminescent material adopts the traditional high-temperature solid phase method of fluorescent powder and adopts the high-temperature solid phase method to synthesize the product of the invention, and the prepared product has the advantages of excellent grain growth quality, less surface defects, loose product, easy crushing, easy scale enlargement and mass production and no influence on the luminescent performance.
In order to achieve the above technical effects, the present application provides the following technical solutions:
in a first aspect, the present invention provides an ultra-wideband green-emitting phosphate luminescent material, which is rare earth Eu 2+ An ion-doped basic phosphate of formula K 3-x La 1-m Ca m (PO 4 ) 2 :xEu 2 + In the formula, x is more than 0 and less than or equal to 0.05, and m is more than or equal to 0 and less than or equal to 0.10.
K 3 La(PO 4 ) 2 Belongs to a natural monopotassium mirabilite mineral structure, and the research on luminescent materials which are used as substrates focuses on the luminescent property after trivalent rare earth ions are doped. The invention designs multi-site aliovalent substitution by rare earth Eu 2+ As luminescent ions, aliovalent substituted monovalent alkali metals K + Ion to obtain ultra-wideband green phosphate K 3 La(PO 4 ) 2 :Eu 2+ A light-emitting material; additional introduction of non-parent component Ca 2+ Ion second aliovalent substitution of La 3+ The ions improve the luminous intensity and quantum efficiency of the green light material, improve the thermal stability and enable the green light material to be more matched with LED application.
The ultra-wideband green light emitting phosphate luminescent material can absorb 250-420nm (near) ultraviolet light, and obtains the ultra-wideband green light emitting fluorescent material with two obvious emission peaks under the excitation of 325nm ultraviolet light, wherein the emission peak range covers 380-700nm, and the half-peak width is 142nm.
In a second aspect, the present invention provides a method for preparing a broadband green light emitting phosphate luminescent material, comprising the steps of:
according to the formula K 3-x La 1-m Ca m (PO 4 ) 2 :xEu 2+ In the formula, x is more than 0 and less than or equal to 0.05, m is more than or equal to 0 and less than or equal to 0.10, oxides containing elements K, la, ca, P and Eu or corresponding salts are used as raw materials for preparing materials, the raw materials are put into a mortar to be mixed with absolute ethyl alcohol, and the materials are fully ground to obtain mixed powder; the obtained mixed powder is put into an alumina crucible to be heated under the reducing atmosphere and is kept warm for a period of time; after cooling to room temperature, the fired sample was taken out and ground.
Verified and prepared K 3-x La(PO 4 ) 2 :xEu 2+ The luminescent material is excited at 250-380nm to obtain ultra-wideband green light emitting fluorescent material with two obvious emission peaks, in series K 3-x La(PO 4 ) 2 :xEu 2+ Of the products, the x =0.02 product has the strongest luminous intensity.
Verified part La 3+ Quilt Ca 2+ The improvement of quantum yield, the enhancement of emission intensity and thermal stability are realized after the aliovalent substitution, and when m =0.05, the quantum efficiency is improved from 25.97% to 55.25%. When m =0.1, the thermal stability rose from 55.1% to 80.2%.
Further, the K-containing oxide or corresponding salt is selected from K 2 O、KNO 3 、K 2 CO 3 (ii) a Preferably K 2 CO 3 。
Further, the La-containing oxide or corresponding salt is selected from La 2 O 3 、La 2 (CO 3 ) 3 (ii) a Preferably La 2 O 3 。
Further, the Ca-containing oxide or corresponding salt is selected from CaO, caCO 3 (ii) a Preferably CaCO 3 。
Further, the oxide containing P or corresponding salt is selected fromFrom NH 4 H 2 PO 4 、(NH 4 ) 2 HPO 4 (ii) a Preferably NH 4 H 2 PO 4 。
Further, the Eu-containing oxide or corresponding salt is selected from Eu 2 O 3 Eu (NO 3) 3; preferably Eu 2 O 3 。
Further, the reducing atmosphere is 10% by volume H 2 And 90% by volume 2 And (4) forming.
Further, the heating temperature is 1000 ℃, and the heat preservation time is 6 hours.
The invention has the beneficial effects that:
(1) The invention selects K 3 La(PO 4 ) 2 As a base material, eu 2+ The ultra-wideband green light emitting luminescent material is prepared by adopting a traditional high-temperature solid phase method for activating ions and is used for eliminating the green light gap phenomenon, the emission peak range of the material covers 380-700nm, the half-peak width is 142nm, and the defect of the traditional fluorescent material in the green light of 480-520nm is made up. In the preparation of K 3 La(PO 4 ) 2 :Eu 2+ In the luminescent material, the quantum yield is improved by using a bialiovalent substitution strategy, and the emission intensity and the thermal stability are enhanced.
(2) The product of the invention is synthesized by a high-temperature solid phase method, and the prepared product has good grain growth quality, few surface defects, loose product, easy crushing, easy scale enlargement and mass production and no influence on the luminescence property.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is K 3-x La(PO 4 ) 2 :xEu 2+ Excitation and emission spectra for x =0.01,0.02,0.04,0.05.
FIG. 2 is K 2.98 La(PO 4 ) 2 :0.02Eu 2+ X-ray diffraction pattern (upper) of sample and standard card PDF #7Comparison of 8-0388 (bottom).
FIG. 3 is K 2.98 La 1-m Ca m (PO 4 ) 2 :0.02Eu 2+ Comparison of the X-ray diffraction pattern of the sample (top) with standard card PDF #78-0388 (bottom).
FIG. 4 is K 2.98 La 1-m Ca m (PO 4 ) 2 :0.02Eu 2+ Emission spectrum of the sample.
FIG. 5 shows K2.98La1-mCam (PO 4) 2 2+ Absolute Quantum Yield (QY) plot of samples.
FIG. 6 shows K 2.98 La 1-m Ca m (PO 4 ) 2 :0.02Eu 2+ Three-dimensional temperature-dependent emission spectra of samples: (a) m =0, (b) m =0.1.
FIG. 7 is K 2.98 La 0.9 Ca 0.1 (PO 4 ) 2 :0.02Eu 2+ Chromaticity coordinate plot of the sample.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1: k 3 La 1-m Ca m (PO 4 ) 2 :xEu 2+ Take m =0, x =0.01,0.02,0.04,0.05.
0.4146 g K are weighed out 2 CO 3 0.4601 g NH 4 H 2 PO 4 0.3258 g La 2 O 3 And 0.0035 (x = 0.01), 0.0070 (x = 0.02), 0.0141 (x = 0.04), 0.0176 (x = 0.05) grams Eu 2 O 3 And putting the mixture into a mortar to be mixed with a certain amount of absolute ethyl alcohol, and fully grinding the mixture to obtain the mixed powder. Charging the resulting mixed powder into an alumina crucible at 10% 2 /90％N 2 Heating to 1000 ℃ under a reducing atmosphere, and keeping the temperature for 6 hours. And cooling to room temperature, taking out the fired sample, and grinding to obtain the ultra-wideband green light emitting luminescent material. Obtained according to the technical scheme of example 1 at 325nm excited to emit light with a spectrum like that of the green light emitting material of fig. 1. The most intense light emitted is the x =0.02 embodiment; FIG. 2 is a comparison of the X-ray powder diffraction pattern of a sample of X =0.02 material prepared according to the protocol of this example with standard card PDF #78-0388, showing that the material prepared is K 3 La(PO 4 ) 2 Pure phase.
Example 2: k 3 La 1-m Ca m (PO 4 ) 2 :xEu 2+ (ii) a Take x =0.02, m =0.05,0.1.
0.4146 g K was weighed out 2 CO 3 0.4601 g NH 4 H 2 PO 4 0.3095, 0.2932 g La 2 O 3 0.01 (m = 0.05), 0.02 (m = 0.10) g CaCO 3 And 0.007 g Eu 2 O 3 And putting the mixture into a mortar to be mixed with a certain amount of absolute ethyl alcohol, and fully grinding the mixture to finally obtain mixed powder. Charging the resulting mixed powder into an alumina crucible at 10% H 2 /90％N 2 Heating to 1000 ℃ under a reducing atmosphere, and keeping the temperature for 6 hours. And cooling to room temperature, taking out the fired sample, and grinding to obtain the ultra-wideband green light emitting luminescent material with optimized performance. Referring to FIG. 3, ca was introduced 2+ The X-ray diffraction pattern of the ionic material sample still showed that the prepared material was in pure phase; referring to FIG. 4, ca 2+ The introduction of ions does not cause the change of the spectrum type, the material still emits green light, but the emission intensity of the ultra-wideband green light phosphate luminescent material is improved; referring to FIG. 5, ca 2+ The introduction of ions improves the quantum yield of the ultra-wideband green phosphate luminescent material; referring to FIG. 6, ca 2+ Introduction of ions compared to no introduction of Ca 2+ The ionic material improves the thermal stability of the ultra-wideband green phosphate luminescent material. Fig. 7 is a color coordinate diagram of the sample with m =0.05, confirming that the material is a green luminescent material.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made to the present application by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (15)
1. An ultra-wideband green-emitting phosphate luminescent material, characterized in that the ultra-wideband green-emitting phosphate luminescent material is rare earth Eu 2+ An ion-doped basic phosphate of the formula K 3-x La 1-m Ca m (PO 4 ) 2 :xEu 2+ In the formula, x is more than 0 and less than or equal to 0.05, and m is more than 0 and less than or equal to 0.10.
2. The ultra-wideband green-emitting phosphate luminescent material according to claim 1, wherein x =0.02 and m =0.05.
3. A method for preparing an ultra-wideband green-emitting phosphate luminescent material according to claim 1 or 2, characterized in that it is represented by formula K 3-x La 1-m Ca m (PO 4 ) 2 :xEu 2+ Wherein x is more than 0 and less than or equal to 0.05, m is more than or equal to 0 and less than or equal to 0.10, oxides containing elements K, la, ca, P and Eu or corresponding salts are used as raw materials for proportioning, the raw materials are put into a mortar to be mixed with absolute ethyl alcohol, and the raw materials are fully ground to obtain mixed powder; putting the obtained mixed powder into an alumina crucible, heating in a reducing atmosphere and preserving heat for a period of time; after cooling to room temperature, the fired sample was taken out and ground.
4. The method of claim 3, wherein the K-containing oxide or corresponding salt is selected from K 2 O、KNO 3 、K 2 CO 3 。
5. The method of claim 4, wherein the K-containing oxide or corresponding salt is K 2 CO 3 。
6. The method according to claim 3, wherein the La-containing oxide or corresponding salt is La 2 O 3 、La 2 (CO 3 ) 3 。
7. The method according to claim 6, wherein the La-containing oxide or corresponding salt is La 2 O 3 。
8. The method according to claim 3, wherein the Ca-containing oxide or corresponding salt is selected from CaO, caCO 3 。
9. The method of claim 8, wherein the Ca-containing oxide or the corresponding salt is CaCO 3 。
10. The process according to claim 3, wherein the P-containing oxide or corresponding salt is selected from NH 4 H 2 PO 4 、(NH 4 ) 2 HPO 4 。
11. The method according to claim 10, wherein the P-containing oxide or corresponding salt is NH 4 H 2 PO 4 。
12. The method according to claim 3, wherein the Eu-containing oxide or corresponding salt is selected from Eu 2 O 3 、Eu(NO3) 3 。
13. The method according to claim 12, wherein the Eu-containing oxide or corresponding salt is Eu 2 O 3 。
14. The method of claim 3, wherein the reducing atmosphere is determined by a volume percent of 10% 2 And 90% by volume 2 And (4) forming.
15. The method according to claim 3, wherein the heating temperature is 1000 ℃ and the holding time is 6 hours.
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