CN111170740A - A kind of high-efficiency red phosphor without thermal quenching and preparation method thereof - Google Patents
A kind of high-efficiency red phosphor without thermal quenching and preparation method thereof Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000010791 quenching Methods 0.000 title claims abstract description 14
- 230000000171 quenching effect Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 39
- 150000002500 ions Chemical class 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 28
- 238000000227 grinding Methods 0.000 claims description 17
- -1 lanthanum ions Chemical class 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 229910001940 europium oxide Inorganic materials 0.000 claims description 5
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 5
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 5
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 229910052706 scandium Inorganic materials 0.000 claims description 4
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 4
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000395 magnesium oxide Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000009877 rendering Methods 0.000 description 3
- 239000012856 weighed raw material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 102100034013 Gamma-glutamyl phosphate reductase Human genes 0.000 description 1
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
- 101001133924 Homo sapiens Gamma-glutamyl phosphate reductase Proteins 0.000 description 1
- 241001085205 Prenanthella exigua Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
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Abstract
本发明属于发光材料领域，具体涉及一种无热猝灭的高效红色荧光粉及其制备方法。所述红色荧光粉的化学组成表示式为La1‑xEuxSc3(BO3)4，其中x为掺杂浓度，0<x≤1，该红色荧光粉为碳酸钙镁石结构，该结构特征在于La离子之间被[BO3]三角体和[ScO6]八面体填充，因此La离子之间的距离较远，有效避免了Eu3+之间的相互作用。本发明提供的红色荧光粉临界掺杂浓度高达80%，量子效率高达88.3%，具有较高的亮度，且发光亮度即使在300℃的高温下也没有衰减，所述荧光粉发光性能优异，制备过程简单，易于工业化生产，可适用于高温环境下或者大功率LED器件，具有巨大的应用前景。
The invention belongs to the field of luminescent materials, in particular to a high-efficiency red fluorescent powder without thermal quenching and a preparation method thereof. The chemical composition of the red phosphor is expressed as La 1-x Eu x Sc 3 (BO 3 ) 4 , where x is the doping concentration, 0<x≤1, the red phosphor is a magnesia carbonate structure, and the The structural feature is that the La ions are filled with [BO 3 ] triangles and [ScO 6 ] octahedra, so the distance between La ions is far away, which effectively avoids the interaction between Eu 3+ . The red fluorescent powder provided by the invention has a critical doping concentration of up to 80%, a quantum efficiency of up to 88.3%, high brightness, and no attenuation of the luminous brightness even at a high temperature of 300° C. The fluorescent powder has excellent luminescence performance and is prepared The process is simple, the industrial production is easy, and it can be applied to high-temperature environments or high-power LED devices, and has huge application prospects.
Description
Technical Field
The invention belongs to the field of luminescent materials, and particularly relates to efficient red fluorescent powder without thermal quenching and a preparation method thereof.
Background
The current white light LED realization scheme mainly adopts YAG to Ce3+The yellow fluorescent powder is coated on a blue light chip to realize a bright white light LED, however, with the popularization of the white light LED, the white light LED is found to have low color rendering index, higher color temperature and luminescent property due to the lack of red components, so that the application range of the white light LED is limited. Therefore, researchers at home and abroad develop a three-primary-color scheme, namely near ultraviolet (NUV, 370-410 nm) chips are utilized to combine RGB three-primary-color (red, green and blue) fluorescent powder, and the scheme has the advantages of high excitation energy, high brightness, high light efficiency, stable color and wide fluorescent powder selectivity and is obvious. However, compared with the mature blue powder and green powder, the red powder is still relatively deficient, so that the research on the red fluorescent powder with excellent luminescence performance becomes a hotspot.
Eu3+Ions are important rare earth ions, and because of their special electron shell structure, they have relatively stable emission color, and are widely used in research and development of red phosphors. To increase Eu3+The absorption efficiency of ions, researchers developed a series of red phosphors with high doping concentration, but after the doping concentration was increased, Eu was added3+The distance between ions is shortened, the interaction is enhanced, and the decrease in luminous efficiency and thermal stability is liable to be caused (ACS Applied Materials and interfaces, 2018, 10(48): 41479-41486, ACS Applied Materials&Interfaces,2016, 8(46): 31772-31782.). Especially, the thermal stability of the fluorescent powder is very important for the performance of modern compact LED devices or high-power LED devices, because the working temperature of the semiconductor devices can reach 150 ℃ or even higher, and the LED devices applied to the fields of deep well exploration, nuclear energy and the like have more strict requirements on the thermal stability of the fluorescent powder, the development of the near ultraviolet excited red fluorescent powder with high brightness, high efficiency and high thermal stability still has great challenges.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the efficient red fluorescent powder without thermal quenching, which has high brightness, high color purity, wide application range and stable performance, and the preparation method thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows: a high-efficiency red fluorescent powder without thermal quenching is characterized in that: the chemical formula of the red fluorescent powder is La1-xEuxSc3(BO3)4Wherein x is the doping concentration, 0<x≤1。
The chromaticity coordinates of the red fluorescent powder are (0.6649-0.6665, 0.3333-0.3348).
The red fluorescent powder is of a calcium carbonate magnesium stone structure, and La ions in the structure are bonded by [ BO ]3]Trigonal sum [ ScO ]6]And (4) filling octahedron.
The preparation method of the non-thermal quenching efficient red fluorescent powder is characterized by comprising the following steps:
the method comprises the following steps: la, Eu, Sc, B = (1-x) x, 3, 4, wherein 0<x is less than or equal to 1, and La containing lanthanum ions is weighed3+Compound raw material of (1), europium ion Eu3+Compound raw material of (1), scandium ion-containing Sc3+Compound raw material of (2), boron ion B3+Grinding and mixing the compound raw materials to obtain mixed powder;
step two: putting the mixed powder obtained in the first step into an agate mortar for grinding for 30min, uniformly mixing, putting into a dried corundum crucible, and presintering at 900-1100 ℃ for 6-10 h;
step three: and (3) putting the mixed powder subjected to the pre-sintering in the step two into an agate mortar for continuously grinding for 30min, continuously calcining at 1300 ℃ after uniform mixing, keeping the temperature for 6h, cooling along with the furnace to obtain a fluffy block sample with light pink color, and grinding the fluffy block sample to obtain the final red fluorescent powder.
The La containing lanthanum ions3+The compound of (A) is lanthanum oxide containing europium ion Eu3+Is europium oxide and contains scandium ions Sc3+The compound of (a) is scandium oxide, and the boron ion B is contained3+The compound of (a) is boric acid.
Compared with the prior art, the technical scheme of the invention has the advantages that:
(1) the fluorescent powder in the invention is Eu3+Ion substituted La3+Ions, which are substituted in the same valence state and have small size difference, do not generate lattice defects;
(2) luminescence center Eu in the invention3+The ions are positioned in the distorted prism polyhedron without inversion symmetry centers, and the electric dipole transition intensity is higher;
(3) the chromaticity coordinate of the red fluorescent powder is very close to the standard red light coordinate (0.67, 0.33) of NTSC, and the purity of the red light is more than 97 percent;
(4) nearest neighbor Eu in the present invention3+The distance between ions is far, so that high-concentration doping (80%) can be tolerated, and the quantum efficiency of 88.3% can be displayed on the basis of the doping;
(5) the red fluorescent powder has ultrahigh heat quenching resistance, and the brightness is not attenuated even at the temperature of 300 ℃;
(6) the red fluorescent powder, the commercial blue fluorescent powder and the commercial green fluorescent powder can be combined to package a high-quality white light LED, the color rendering index Ra of the white light LED is as high as 92.5, and the color temperature CCT of the white light LED is as low as 3438K.
The high-brightness borate red fluorescent powder LaSc prepared by the invention3(BO3)4:Eu3+The preparation method is simple, environment-friendly and pollution-free, and is easy for industrial production, so that the preparation method has wide market prospect.
Drawings
FIG. 1 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+The crystal structure of (a);
FIG. 2 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+comprises β -LaSc3(BO3)4A standard X-ray diffraction pattern (ICSD No. 89013);
FIG. 3 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+And commercial red phosphor CaAlSiN3:Eu2+The excitation spectrum of (1);
FIG. 4 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+And commercial red phosphor CaAlSiN3:Eu2+The emission spectrum of (a);
FIG. 5 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+The quantum efficiency test spectrogram;
FIG. 6 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+A change in luminous intensity in the range of 0-300 ℃;
FIG. 7 shows LaSc of a red phosphor sample in example 13(BO3)4:Eu3+And commercial blue phosphor BaMgAl10O17:Eu2+And green phosphor (Ca, Sr)2SiO4:Eu2+An electroluminescence spectrogram of the warm white light LED constructed by combining the 395 nm near ultraviolet LED chip;
FIG. 8 is the XRD structure refinement pattern of the red phosphor sample in example 3, the refinement templates respectively adopt α -LaSc3(BO3)4(ICSD No. 83404) and β -LaSc3(BO3)4(ICSD No. 89013), and the refinement software was GSAS.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description of the specific embodiments, methods, steps, features and effects of the non-thermal quenching efficient red phosphor and the preparation method thereof according to the present invention with reference to the preferred embodiments is as follows:
example 1:
according to the chemical formula La0.2Eu0.8Sc3(BO3)4Respectively weighing 0.0977g of lanthanum oxide, 0.4223g of europium oxide, 0.6206g of scandium oxide and 0.7643g of boric acid according to the stoichiometric ratio of each element, and putting the weighed raw materials into an agate mortar for grinding for 0.5 hour to obtain the mixtureUniformly mixing, putting the obtained mixture into a dried corundum crucible, putting the crucible into a muffle furnace, pre-burning at 1100 ℃, preserving heat for 6 hours, grinding and uniformly mixing the pre-burned mixture, continuously calcining at 1300 ℃, preserving heat for 6 hours, naturally cooling with the furnace to obtain a light pink blocky product, grinding the blocky product to obtain the final La blocky product0.2Eu0.8Sc3(BO3)4the chromaticity coordinate of the red phosphor is (0.6661, 0.3336), and the X-ray diffraction analysis of the red phosphor shows that the crystal phase is mainly β -LaSc3(BO3)4The structural phase (as shown in figure 2), the fluorescence spectrometer detection result shows that the excitation intensity and the emission intensity are far greater than those of the commercial nitride red fluorescent powder CaAlSiN3:Eu2+(as shown in FIGS. 3 and 4), and the emission spectrum is narrower, the quantum yield is up to 88.3% (as shown in FIG. 5), and the fluorescent powder has ultrahigh thermal stability, and the luminescence does not fade (as shown in FIG. 6) even under the severe environment of 300 ℃, and is similar to the commercial blue fluorescent powder BaMgAl10O17:Eu2+And green phosphor (Ca, Sr)2SiO4:Eu2+The warm white LED device constructed in combination with the 395 nm near ultraviolet LED chip exhibits the advantages of high color rendering index and low color temperature (as shown in FIG. 7).
Example 2:
according to the chemical formula La0.4Eu0.6Sc3(BO3)4Respectively weighing 0.1955g of lanthanum oxide, 0.3167g of europium oxide, 0.6206g of scandium oxide and 0.7643g of boric acid according to the stoichiometric ratio of the elements, putting the weighed raw materials into an agate mortar for grinding for 0.5 hour to obtain a uniform mixture, putting the obtained mixture into a dry corundum crucible, putting the crucible into a muffle furnace, presintering at 1000 ℃, preserving heat for 8 hours, grinding and uniformly mixing the presintered mixture, continuously calcining at 1300 ℃, preserving heat for 6 hours, naturally cooling along with the furnace to obtain a light pink blocky product, grinding the blocky product to obtain the final La blocky product0.4Eu0.6Sc3(BO3)4And (4) red fluorescent powder. The chromaticity coordinate of the red phosphor is (0.6662, 0.3335), and the red phosphor is detectedthe crystal phase is mainly β -LaSc3(BO3)4The structure is similar to that of example 1.
Example 3:
according to the chemical formula EuSc3(BO3)40.5279g of europium oxide, 0.6206g of scandium oxide and 0.7643g of boric acid are respectively weighed according to the stoichiometric ratio of each element in the formula; putting the weighed raw materials into an agate mortar for grinding for 0.5 hour to obtain a uniform mixture, putting the obtained mixture into a dry corundum crucible, putting the crucible into a muffle furnace, presintering at 900 ℃, preserving heat for 10 hours, grinding and uniformly mixing the presintered mixture, continuously calcining at 1300 ℃, preserving heat for 6 hours, naturally cooling along with the furnace to obtain a light pink blocky product, grinding the blocky product to obtain the final EuSc3(BO3)4the chromaticity coordinate of the red phosphor is (0.6663, 0.3335), and the detected crystal phase of the red phosphor is mainly α -LaSc3(BO3)4structural phase sum β -LaSc3(BO3)4the emission spectrum shape was similar to that of example 1 with the mixed phases of the structural phases having alpha and β phases contents of 13.54% and 86.46%, respectively (as shown in fig. 8).
Claims (5)
1. A high-efficiency red fluorescent powder without thermal quenching is characterized in that: the chemical formula of the red fluorescent powder is La1- xEuxSc3(BO3)4Wherein x is the doping concentration, 0<x≤1。
2. The non-thermal quenching high efficiency red phosphor according to claim 1, wherein: the chromaticity coordinates of the red fluorescent powder are (0.6649-0.6665, 0.3333-0.3348).
3. The non-thermal quenching high efficiency red phosphor according to claim 1, wherein: the red fluorescent powder is of a calcium carbonate magnesium stone structure, and La ions in the structure are bonded by [ BO ]3]Trigonal sum [ ScO ]6]And (4) filling octahedron.
4. The method for preparing efficient red fluorescent powder without thermal quenching as claimed in claim 1, comprising the steps of:
the method comprises the following steps: la, Eu, Sc, B = (1-x) x, 3, 4, wherein 0<x is less than or equal to 1, and La containing lanthanum ions is weighed3+Compound raw material of (1), europium ion Eu3+Compound raw material of (1), scandium ion-containing Sc3+Compound raw material of (2), boron ion B3+Grinding and mixing the compound raw materials to obtain mixed powder;
step two: putting the mixed powder obtained in the first step into an agate mortar for grinding for 30min, uniformly mixing, putting into a dried corundum crucible, and presintering at 900-1100 ℃ for 6-10 h;
step three: and (3) putting the mixed powder subjected to the pre-sintering in the step two into an agate mortar for continuously grinding for 30min, continuously calcining at 1300 ℃ after uniform mixing, keeping the temperature for 6h, cooling along with the furnace to obtain a fluffy block sample with light pink color, and grinding the fluffy block sample to obtain the final red fluorescent powder.
5. The method for preparing efficient red fluorescent powder without thermal quenching as claimed in claim 4, wherein: the La containing lanthanum ions3+The compound of (A) is lanthanum oxide containing europium ion Eu3+Is europium oxide and contains scandium ions Sc3+The compound of (a) is scandium oxide, and the boron ion B is contained3+The compound of (a) is boric acid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111057546A (en) * | 2020-01-15 | 2020-04-24 | 中山大学 | A kind of Eu3+ activated red phosphor with high quantum yield and preparation method thereof |
| CN112500853A (en) * | 2020-12-14 | 2021-03-16 | 新沂市锡沂高新材料产业技术研究院有限公司 | Ce3+Doped zero-thermal quenching fluorescent powder and preparation method thereof |
| CN115074127A (en) * | 2022-07-06 | 2022-09-20 | 中山大学 | Borate based on divalent europium ion and trivalent europium ion co-activation, and preparation method and application thereof |
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| CN108998025A (en) * | 2018-07-31 | 2018-12-14 | 景德镇陶瓷大学 | A kind of LED silicate-base red fluorescence powder and preparation method thereof |
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