WO2022233116A1 - Poudre fluorescente à double émission à matrice unique, procédé de préparation associé et utilisation correspondante - Google Patents
Poudre fluorescente à double émission à matrice unique, procédé de préparation associé et utilisation correspondante Download PDFInfo
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- WO2022233116A1 WO2022233116A1 PCT/CN2021/128249 CN2021128249W WO2022233116A1 WO 2022233116 A1 WO2022233116 A1 WO 2022233116A1 CN 2021128249 W CN2021128249 W CN 2021128249W WO 2022233116 A1 WO2022233116 A1 WO 2022233116A1
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- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 8
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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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G7/00—Botany in general
- A01G7/04—Electric or magnetic or acoustic treatment of plants for promoting growth
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
- F21V9/30—Elements containing photoluminescent material distinct from or spaced from the light source
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/14—Measures for saving energy, e.g. in green houses
Definitions
- the present invention relates to the technical field of luminescent materials, and more particularly, to a single-matrix double-emitting phosphor and a preparation method and application thereof.
- Light is the basic factor of plant growth and development. It can not only provide the energy required for photosynthesis of plants, but also regulate plant life activities, such as seed germination, seedling formation, flowering and fruiting and other processes. At the same time, greenhouse planting and environment-controlled indoor planting have attracted much attention as a method of environmental protection, energy saving and sustainable development. It can be seen that plant lighting technology is an indispensable part of modern agricultural construction, especially for the lack of land resources. For areas with light conditions and light conditions, plant light is particularly important. Studies have shown that photoreceptors of plants dominate many processes of metabolism and growth and development of plants, and the response spectral ranges are mainly concentrated in blue light at 400-500 nm, red light at 600-780 nm and deep red light.
- the emission spectrum of traditional lighting sources does not match the spectrum required for plant growth, resulting in low utilization of light energy, wasting energy, and affecting the effective growth of plants.
- the LED lighting source has the advantages of high luminous efficiency, low heat generation, small size, long life, and the emission spectrum can be adjusted by changing the phosphor composition to match the absorption spectrum required for plant growth. It has advantages in the field of plant lighting. obvious.
- Lead-based halide perovskite materials have good optoelectronic properties and have been used to fabricate devices such as light-emitting diodes, solar cells, and photodetectors.
- the toxicity and chemical instability of lead will pose a fatal threat to life and health and severely limit the service life and application prospects of equipment.
- the use of non-toxic metal ions to replace lead ions in lead halide perovskites can effectively solve the problem of lead-based
- lead-free perovskite phosphors have a narrow excitation spectrum range, and cannot achieve stable and adjustable light color, and cannot meet the matching requirements of the absorption spectrum required for plant growth.
- CN109973842A discloses a preparation method of a long afterglow LED plant lamp light-emitting chip.
- the specific steps of the preparation method are as follows: (1) Phosphor BaMgAl 10 O 17 :Eu 2+ , Sr 2 SiO 4 :Eu 2+ , CaAlSiN: Eu 2+ , SrAl 2 O 4 : Eu 2+ , Dy 3+ , CaAl 2 O 4 : Eu 2+ , Dy 3+ , ZnG a2 O 4 : Cr 3+ , Bi 3+ were dry-milled and mixed for 30 ⁇ Mixed powder A was obtained in 45min; wherein the phosphors BaMgAl 10 O 17 :Eu 2+ , Sr 2 SiO 4 :Eu 2+ , CaAlSiN:Eu 2+ , SrAl 2 O 4 :Eu 2+ ,Dy 3+ ,CaAl 2 O 4 : Eu 2+ , Dy 3+ and Z
- the perovskite material of the long afterglow LED plant lamp light-emitting chip disclosed above is not a single-matrix fluorescent material, and it is mainly aimed at adjusting the illumination brightness of red and blue LED plant lamps to achieve automatic modulation of spectrum, and does not solve the problem of using single-matrix fluorescence.
- the material can realize multi-color tunability, achieve stable wide-spectrum excitation, and meet the requirements of the absorption spectrum required by plants.
- the technical problem to be solved by the present invention is to overcome the defects and deficiencies that the existing perovskite fluorescent materials cannot achieve stable wide-spectrum excitation and emission powder light, and cannot well fit the absorption spectrum required by plants, and provide a single-substrate dual
- the emitting phosphor can realize light color by doping trivalent ions Bi 3+ and Sb 3+ in the single-host lead-free inorganic perovskite Cs 2 SnCl 6 and adjusting the content of trivalent ions Bi 3+ and Sb 3+ It is stable and adjustable, effectively absorbs near-ultraviolet light within 300 ⁇ 400nm, emits red and blue light at 400 ⁇ 525nm and 550 ⁇ 850nm, which matches the absorption spectrum required by plants. The powder light required.
- Another object of the present invention is to provide a method for preparing a single-matrix double-emitting phosphor.
- Another object of the present invention is to provide an application of a single-substrate dual-emitting phosphor in the preparation of plant lighting equipment.
- Another object of the present invention is to provide a plant lighting LED.
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is:
- x and y are the molar percentages of doping ions Bi 3+ and Sb 3+ , respectively, relative to the host ions Sn 4+ .
- the fluorescent powder material of the invention is a single-matrix dual-emission fluorescent powder, and the single-matrix dual-emission fluorescent material only needs a single matrix to emit blue and red two kinds of light, which solves the possible reabsorption caused by the combination of two or more fluorescent materials.
- the different aging rates of various fluorescent materials cause unstable light color, and the proportion of various fluorescent powders is complicated.
- the host material of the single-host double-emitting fluorescent material is lead-free all-inorganic perovskite Cs 2 SnCl 6 , and the light-emitting centers are respectively trivalent ions Bi 3+ and Sb 3+ .
- the trivalent ion Bi 3+ emits blue light in the matrix, with an emission peak at 400-525 nm, and Sb 3+ produces red light with an emission peak at 550-850 nm, which is in line with the absorption spectrum required by plants.
- the two light colors are mixed to obtain pink light that meets the needs of plant lighting.
- the single-host dual-emitting fluorescent material of the present invention can obtain a dual-emitting fluorescent powder with adjustable light color by changing the doping ratio of trivalent ions Bi 3+ and Sb 3+ and selecting different ratios within a certain range.
- the doping ratio of Bi 3+ and Sb 3+ By adjusting the doping ratio of Bi 3+ and Sb 3+ , the ratio of blue light and red light can be effectively adjusted, and the pink light required for plant growth can be obtained.
- different plant species and different growth cycles in the plant growth process require different light colors, so an adjustable light source with a suitable blue-red ratio is required to meet different needs.
- the phosphor material of the present invention can pass Bi 3+ , Sb The adjustment of the doping ratio of 3+ can realize the adjustment of different light sources.
- the dual emission fluorescent material of the present invention Due to the doping of Bi 3+ and Sb 3+ ions, the dual emission fluorescent material of the present invention has a very wide excitation spectrum, has effective absorption in the range of 300-400 nm, and can effectively absorb the near-ultraviolet emitted by the ultraviolet LED chip.
- the light emits blue and red light at 400-525nm and 550-850nm, and can be adjusted to obtain the required light source.
- Reabsorption is when the emission spectrum of one phosphor overlaps the excitation spectrum of another phosphor, resulting in a decrease in the former's luminescence.
- the excitation spectrum of the blue-red light of the single-host dual-emission fluorescent material of the present invention is both at 300-400 nm, and the excitation and emission spectra of the two do not overlap, which can avoid reabsorption.
- the luminescence center is in the same matrix, the luminescence of the material has a similar aging rate, which reduces the problem of unstable composite light color caused by different aging rates of different phosphor materials.
- the single-matrix double-emitting fluorescent material of the present invention avoids the re-absorption effect of the composite of various fluorescent powders, and reduces the instability of the composite light color caused by the different aging rates of the various fluorescent powders, and the complex adjustment of the ratio of different fluorescent powders, etc. question. Avoiding re-absorption in applications can make more efficient use of the excitation energy of LEDs.
- the stability of light color means that the ratio of luminous peaks remains unchanged, which better maintains the stability of the energy of light absorbed by plants. Scale preparation.
- the content of fixed Sb ions is 0.15, and the content of Bi ions is changed between 0.005 and 0.09, and the relative intensity of the red and blue emission peaks of the sample will change accordingly, so that the light color can be adjusted, and the light from red to blue can be obtained. , to meet the requirements of plant LED lighting for different light colors at different stages of plant growth.
- the content of fixed Bi ions is 0.09, and the content of Sb ions is changed between 0.05 and 0.25, and the relative intensities of the red and blue emission peaks of the sample will change accordingly, and the light from blue to red can be adjusted to achieve adjustable light color. , to meet the requirements of plant LED lighting for different light colors at different stages of plant growth
- the present invention also specifically protects a method for preparing the above-mentioned single-substrate dual-emitting phosphor, comprising the following steps:
- the preparation process of the pink fluorescent material in the present invention is simple, easy to implement, low in cost, low in toxicity, and has broad prospects for large-scale industrial application.
- the Cs-containing compound is Cs oxide, Cs carbonate, Cs hydroxide, Cs nitrate or Cs chloride;
- the Sn-containing compound is Sn oxide, Sn carbonate, Sn hydroxide, Sn nitrate or Sn chloride;
- the Bi-containing compound is Bi oxide, Bi carbonate, Bi hydroxide, Bi nitrate or Bi chloride;
- the Sb-containing compound is an oxide of Sb, a carbonate of Sb, a hydroxide of Sb, a nitrate of Sb, or a chloride of Sb.
- Chloride can provide both cations and anions required for the reaction, which is better for the preparation of pure phases. Therefore, further preferably, the Cs-containing compound is Cs chloride; the Sn-containing compound is Sn chloride; the Bi-containing compound is Bi chloride; the Sb-containing compound is Sb chloride matter.
- the cooling is cooling to room temperature at a rate of 10-30°C/1h.
- the control of the cooling rate can better achieve the high luminous efficiency of the material.
- the single-substrate dual-emitting fluorescent powder of the invention has wide-spectrum excitation, can effectively absorb and emit powder light in the near-ultraviolet light spectrum that fits the absorption band of plants, and at the same time realizes light color adjustment, and can be widely used in fluorescent powder light color adjustment.
- the invention particularly specifically protects the application of the above-mentioned single-substrate dual-emitting phosphor in the preparation of plant lighting equipment.
- the ultraviolet LED chip of the plant lighting device in the application has an emission wavelength of 300 nm to 400 nm, more preferably 365 nm.
- the present invention also specifically protects a plant lighting LED, which is prepared by encapsulating the single-substrate dual-emitting phosphor powder and an ultraviolet LED diode chip.
- the dual-emission fluorescent material of the present invention is doped with trivalent ions Bi 3+ and Sb 3+ , and the emission peaks are located at 400-525 nm (Bi 3+ ) and 550-850 nm (Sb 3+ ), respectively, which are similar to those of plants.
- the required absorption spectrum is matched, and the content of trivalent ions Bi 3+ and Sb 3+ can be adjusted to achieve stable and adjustable light color, and obtain the pink light required for plant growth.
- the dual emission fluorescent material of the present invention has a very wide excitation spectrum, can effectively absorb in the range of 300-400 nm, and can effectively absorb the near-ultraviolet light emitted by the ultraviolet LED chip.
- the dual emission fluorescent material of the present invention is a single matrix material, which can effectively avoid reabsorption, unstable light color caused by different aging rates, and The complex ratio adjustment and other problems can make the light color stable and not produce large color drift.
- the preparation process of the pink fluorescent material of the present invention is simple, easy to realize, low in cost and low in toxicity, and can be applied in large-scale industrialization.
- FIG. 1 is the XRD patterns of the single-matrix double-emitting phosphors of Examples 1-4.
- FIG. 2 is the XRD patterns of the single-matrix double-emitting phosphors of Examples 5-8.
- 3 is an emission spectrum diagram of the single-matrix double-emitting phosphors of Examples 1-4.
- FIG. 5 is an emission spectrum diagram of the single-matrix dual-emitting phosphor of Example 3.
- FIG. 6 is an excitation spectrum diagram of monitoring different emission wavelength positions of the single-matrix dual-emitting phosphor of Example 3.
- FIG. 6 is an excitation spectrum diagram of monitoring different emission wavelength positions of the single-matrix dual-emitting phosphor of Example 3.
- the raw material reagents used in the examples of the present invention are conventionally purchased raw material reagents.
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.845 Bi 0.005 Sb 0.15 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.843 Bi 0.007 Sb 0.15 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.845 Bi 0.01 Sb 0.15 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.845 Bi 0.048 Sb 0.15 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.86 Bi 0.09 Sb 0.05 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.81 Bi 0.09 Sb 0.1 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.81 Bi 0.09 Sb 0.15 Cl 6 .
- the preparation method is as follows:
- a single-matrix double-emission phosphor the chemical formula of the single-matrix double-emission phosphor is: Cs 2 Sn 0.845 Bi 0.09 Sb 0.25 Cl 6 .
- the preparation method is as follows:
- Fig. 1 is the XRD patterns of Examples 1-4.
- the XRD patterns of the phosphors prepared in Examples 1-4 are basically consistent with the standard card (ICSD#9023), which further confirms the purity of the phosphors prepared in Examples 1-4 of the present application. high.
- Fig. 2 is the XRD patterns of Examples 5-8.
- the XRD patterns of the phosphors prepared in Examples 5-8 are basically consistent with the standard card (ICSD#9023), which further confirms the purity of the phosphors prepared in Examples 5-8 of the present application. high.
- Fig. 3 and Fig. 4 show that a series of double-emitting phosphor samples with different ion concentrations (the ions are Bi 3+ and Sb 3+ ) obtained according to the preparation method of the present invention (the chemical composition expression is: Cs 2 Sn 1-xy Bi x Sb y Cl 6 , where x and y are the molar percentages of doping ions Bi 3+ , Sb 3+ , relative to host ions Sn 4+ , respectively, the value range: 0.005 ⁇ x ⁇ 0.09, 0.05 ⁇ y ⁇ 0.25) have similar spectral properties.
- Figure 3 shows the emission spectra of the luminescent materials of Examples 1 to 4. It can be seen from Figure 3 that the doping amount of antimony (Sb 3+ ) ions in the sample is fixed, and the doping amount of bismuth (Bi 3+ ) ions in the sample is changed , the relative intensity of the red and blue emission peaks of the sample will change accordingly, so that the light color can be adjusted.
- Sb 3+ antimony
- Bi 3+ bismuth
- Fig. 4 shows the emission spectra of the luminescent materials of Examples 5-8. It can be seen from Fig. 4 that the doping amount of bismuth (Bi 3+ ) ions in the samples is fixed, and the doping amount of antimony (Sb 3+ ) ions in the samples is changed , the relative intensity of the red and blue emission peaks of the sample will change accordingly, so that the light color can be adjusted.
- Figure 5 is the emission spectrum diagram of the luminescent material of Example 3. It can be seen from Figure 5 that the pink fluorescent material has relatively excellent emission in both blue and red light bands under the excitation of 365 nm light, and the emission peaks are respectively located at: 400-525 nm (Bi 3+ ), 550-850 nm (Sb 3+ ), can emit pink light emission matching the absorption spectrum required for plant growth after combining. Chlorophyll A and B are hormones required for plant growth. Figure 5 shows that the emission spectrum of the material matches the absorption of chlorophyll A and B, which is suitable for plant lighting needs.
- Example 6 is the excitation spectrum of the luminescent material of Example 3 monitored at different emission wavelength positions.
- the excitation spectrum exhibits broadband absorption from 300 nm to 400 nm, indicating that the material can meet the excitation requirements of near-ultraviolet LED chips.
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Abstract
La présente invention concerne une poudre fluorescente à double émission à matrice unique, un procédé de préparation associé et une utilisation correspondante, qui appartiennent au domaine technique des matériaux électroluminescents. La poudre fluorescente à double émission à matrice unique a une formule chimique de Cs2Sn1-x-yBixSbyCl6, 0,005≤x≤0,09, et 0,05≤y≤0,25 étant satisfaites. La poudre fluorescente présente un spectre d'excitation très large, peut absorber efficacement la lumière dans la plage de 300 à 400 nm, peut absorber efficacement la lumière proche ultraviolette émise par une puce DEL ultraviolette, et est dopée avec des ions trivalents de Bi3+ et Sb3+. Les spectres d'émission sont respectivement situés à 400-525 nm (Bi3+) et 550-850 nm (Sb3+), tous deux étant alignés avec le spectre d'absorption requis par les plantes. En ajustant la teneur en ces ions trivalents de Bi3+ et Sb3+, une couleur claire stable et ajustable peut être obtenue, et une lumière rose requise pour la croissance des plantes est obtenue, et la poudre fluorescente est un matériau à matrice unique ; et comparé à la préparation d'une DEL d'éclairage de plante par mélange de poudres fluorescentes multicolores, les problèmes de réabsorption, de couleur claire instable, de vitesses de vieillissement différentes, d'un ajustement compliqué du rapport de différentes poudres fluorescentes, etc., peuvent être efficacement évités, et le processus de préparation a un procédé simple, est facile à réaliser, est peu coûteux, a une faible toxicité, et peut être appliqué à une industrialisation à grande échelle.
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CN113355092A (zh) * | 2021-05-07 | 2021-09-07 | 中山大学 | 一种单基质双发射荧光粉及其制备方法与应用 |
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CN107017325A (zh) * | 2015-11-30 | 2017-08-04 | 隆达电子股份有限公司 | 量子点复合材料及其制造方法与应用 |
CN111500288A (zh) * | 2019-01-31 | 2020-08-07 | 隆达电子股份有限公司 | 钙钛矿纳米发光晶体、发光装置及钙钛矿纳米发光晶体的制造方法 |
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