CN113999677B - Dual-band ultraviolet excited red fluorescent powder and preparation method and application thereof - Google Patents
Dual-band ultraviolet excited red fluorescent powder and preparation method and application thereof Download PDFInfo
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- CN113999677B CN113999677B CN202111460792.7A CN202111460792A CN113999677B CN 113999677 B CN113999677 B CN 113999677B CN 202111460792 A CN202111460792 A CN 202111460792A CN 113999677 B CN113999677 B CN 113999677B
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- 239000000843 powder Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 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 abstract description 12
- 238000000295 emission spectrum Methods 0.000 claims abstract description 10
- 239000000049 pigment Substances 0.000 claims abstract description 9
- 230000008635 plant growth Effects 0.000 claims abstract description 8
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229910001940 europium oxide Inorganic materials 0.000 claims abstract description 6
- 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 abstract description 6
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229930002869 chlorophyll b Natural products 0.000 claims abstract description 5
- NSMUHPMZFPKNMZ-VBYMZDBQSA-M chlorophyll b Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C=O)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 NSMUHPMZFPKNMZ-VBYMZDBQSA-M 0.000 claims abstract description 5
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001195 gallium oxide Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 4
- 229940093474 manganese carbonate Drugs 0.000 claims abstract description 3
- 235000006748 manganese carbonate Nutrition 0.000 claims abstract description 3
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 3
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 16
- 230000005284 excitation Effects 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 8
- 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
- 239000011572 manganese Substances 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims 1
- 239000005340 laminated glass Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002985 plastic film Substances 0.000 claims 1
- 229920006255 plastic film Polymers 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 229910052733 gallium Inorganic materials 0.000 abstract description 2
- 238000010413 gardening Methods 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 7
- 230000004907 flux Effects 0.000 description 5
- 238000000695 excitation spectrum Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000012010 growth Effects 0.000 description 3
- 230000029553 photosynthesis Effects 0.000 description 3
- 238000010672 photosynthesis Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241001464837 Viridiplantae Species 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006690 co-activation Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229910001938 gadolinium oxide Inorganic materials 0.000 description 1
- 229940075613 gadolinium oxide Drugs 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000027874 photomorphogenesis Effects 0.000 description 1
- 230000002165 photosensitisation Effects 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 230000027870 phototropism Effects 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
- C09K11/77—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
- C09K11/7784—Chalcogenides
- C09K11/7787—Oxides
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Botany (AREA)
- Ecology (AREA)
- Forests & Forestry (AREA)
- Environmental Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides red fluorescent powder and a preparation method and application thereof. The red fluorescent powder is a compound represented by a formula I: RE (RE) m M a O 3 :bEu 3+ ,cMn 4+ The method comprises the steps of carrying out a first treatment on the surface of the Wherein the RE contains one or two of La, Y, gd, lu and Sc, and the sum of the atomic numbers of the RE elements ismAnd saidmIs in the range of 0<m<1. The M comprises one or two of Al and Ga; the sum of the atomic numbers of the M elements isaAnd saidaIs in the range of 0<a<1. Lanthanum oxide, aluminum hydroxide, gallium oxide, europium oxide and manganese carbonate are used as raw materials, high-temperature solid phase reaction is adopted under the air atmosphere, and 4-6 h is kept at 1400-1600 ℃ in a box-type furnace. The fluorescent powder of the invention has the property of converting B-band ultraviolet light into red light with a main peak of 619 nm and converting A-band ultraviolet light into far-red light with a main peak of 720 nm, and the emission spectrum of the fluorescent powder is respectively matched with plant chlorophyll B and P FR The absorption spectrum of the pigment is overlapped, and when the red fluorescent powder is applied to the gardening or agriculture field, the growth of plants can be promoted.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to red fluorescent powder and a preparation method and application thereof.
Background
Light is not only an energy source for plant growth, but also controls physiological processes such as growth and differentiation of plant cells. The blue light band (400-500 nm), the red light band (600-680 nm) and the far-red light band (680-760 nm) in sunlight correspond to the promotion of photosynthesis, phototropism and photomorphogenesis of plants, respectively. The ultraviolet light is converted into red light and far-red light, so that solar energy can be utilized to the maximum extent for agricultural production.
The influence of light on plants is mainly reflected in illumination time, intensity, light quality and the like. The light quality is an important ring of illumination conditions, the light signals of different light qualities are closely related to the growth and development of plants, the yield and the plant quality, and especially the influence of the ratio (R/FR) of red light (R) to far-red light (FR) luminous flux in a spectrum on the growth and development of plants is more and more emphasized. The growth of plants can be regulated by manually adjusting the luminous flux ratio of red light and far-red light.
In recent years, many researchers have focused on far-red phosphors, and few have studied influencing plant growth by adjusting the luminous flux ratio. In 2020, eu was reported 3+ , Mn 4+ Co-activation K 0.3 La 1.233 MgWO 6 Fluorescent powder (ACS appl. Electron. Mater 2020, 2, 3889-3897) with optimal excitation wavelength in blue light region can be used as LED light source for plant growth. But does not see the use of Eu 3+ , Mn 4+ The fluorescent powder is co-doped to synthesize aluminate fluorescent powder, realizes broadband ultraviolet excitation and broadband red area emission (near red light to far red light area), and is applied to plant cultivation reports.
Disclosure of Invention
In view of the above technical problems, an object of the present invention is to provide a red phosphor, a preparation method and an application thereof, wherein the emission spectrum of the red phosphor is equal to chlorophyll b and photosensitizing pigment P of green plants FR The absorption spectrum is high in matching degree, and the luminous flux ratio of red light (R) and far-red light (FR) can be manually adjusted to promote the growth of plants.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the first aspect of the invention provides a red fluorescent powder, which is a compound represented by a formula I:
RE m M a O 3 :bEu 3+ ,cMn 4+
wherein the M comprises one or both of Al and Ga; the RE comprises one or both of La, Y, gd, lu and Sc;
the sum of the atomic numbers of the elements contained in the M isaAnd saidaIs in the range of 0< a <1, the sum of the atomic numbers of the elements contained in the RE ismAnd saidmIs in the range of 0< m <1。
In some alternative embodiments, the formula I is
RE 1-b Al a-c1- Ga a O 3 :bEu 3+ ,cMn 4+
Wherein the saidbThe range of (2) is 0.04-0b ≤ 0.08，cThe range of (2) is 0.0001-lessc ≤ 0.001。
In some alternative embodiments, the red phosphor is selected from one or more of the following compounds:
La 0.95 Al 0.8 Ga 0.2 O 3 :0.05Eu 3+ ,0.0005Mn 4+
La 0.93 Al 0.7 Ga 0.3 O 3 :0.07Eu 3+ ,0.0005Mn 4+
La 0.75 Gd 0.2 AlO 3 :0.05Eu 3+ ,0.001Mn 4+
in some alternative embodiments, the red phosphor emits a narrow band near red light with peak at 619 nm when excited by light having an ultraviolet wavelength of 329 nm, emits a broad band far red light with peak at 720 nm when excited by light having 373 nm.
In some alternative embodiments, the red color has a wavelength in the range of 600-750 nm.
In a second aspect, the present invention provides a method for preparing a red phosphor according to any one of the above embodiments, comprising the steps of:
mixing and grinding lanthanum oxide, aluminum hydroxide, gallium oxide, europium oxide and manganese carbonate to obtain a mixed solid;
calcining the mixed solid in an air atmosphere to obtain the red fluorescent powder;
wherein the temperature of the calcination is 1400-1600 ℃, and the time of the calcination is 4.0-7.0 h.
Drawings
Fig. 1: x-ray powder diffraction pattern of phosphor of example 2 of the present invention
Fig. 2: excitation Spectrum (monitoring wavelength 619 nm) of the phosphor according to example 2 of the present invention
Fig. 3: the excitation spectrum (monitoring wavelength 720 nm) of the phosphor of example 2 of the present invention
Fig. 4: the phosphor of example 2 of the present invention has an emission spectrum (excitation wavelength 329 nm)
Fig. 5: the phosphor of example 2 of the present invention has an emission spectrum (excitation wavelength 373 nm)
Fig. 6: the fluorescent powder of the embodiment 2 of the invention has an emission spectrum and a plant photosensitive pigment P FR Absorption spectrum contrast of chlorophyll b
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following are non-limiting examples of the phosphor synthesis of the present invention:
example 1
La 0.95 Al 0.8 Ga 0.2 O 3 :0.05Eu 3+ ,0.0005Mn 4+
The embodiment provides a preparation method of red fluorescent powder, which comprises the following steps:
(1) The raw materials are weighed according to the stoichiometric ratio, and the specific implementation is as follows: 7.7380 g lanthanum oxide (La) 2 O 3 ) 3.1202 g aluminium hydroxide (Al (OH) 3 ) 0.9372 g gallium oxide (Ga) 2 O 3 ) Europium oxide (Eu) 0.44. 0.44 g 2 O 3 ) And 0.0029 g manganese carbonate (MnCO 3 ) Uniformly mixing and grinding to obtain mixed powder;
(2) Pouring the mixed powder into an alumina crucible, calcining 5.0. 5.0 h in a box-type high temperature furnace at 1500 ℃, cooling to room temperature, and fully grinding to obtain La 0.95 Al 0.8 Ga 0.2 O 3 :0.05Eu 3+ ,0.0005Mn 4+ Red fluorescent powder.
Example 2
La 0.93 Al 0.7 Ga 0.3 O 3 :0.07Eu 3+ ,0.0005Mn 4+
The embodiment provides a preparation method of red fluorescent powder, which comprises the following steps:
(1) The raw materials are weighed according to the stoichiometric ratio, and the specific implementation is as follows: 7.5751 g lanthanum oxide (La) 2 O 3 ) 2.7301 g aluminium hydroxide (Al (OH) 3 ) 1.4058 g gallium oxide (Ga) 2 O 3 ) Europium oxide (Eu) 0.616 g 2 O 3 ) And 0.0029 g manganese carbonate (MnCO 3 ) Uniformly mixing and grinding to obtain mixed powder;
(2) Pouring the mixed powder into an alumina crucible, calcining 5.0. 5.0 h in a box-type high temperature furnace at 1500 ℃, cooling to room temperature, and fully grinding to obtain La 0.93 Al 0.7 Ga 0.3 O 3 :0.07Eu 3+ ,0.0005Mn 4+ Red fluorescent powder. Under the excitation of ultraviolet light, the fluorescent powder emits red light and far-red light. And the luminous flux can be adjusted manually by changing the composition of the fluorescent powder to promote the growth of plants.
Example 3
La 0.75 Gd 0.2 AlO 3 :0.05Eu 3+ ,0.001Mn 4+
(1) The raw materials are weighed according to the stoichiometric ratio, and the specific implementation is as follows: 6.1089 g lanthanum oxide (La) 2 O 3 ) Gadolinium oxide 1.813 g (Gd) 2 O 3 ) 3.9002 g aluminium hydroxide (Al (OH) 3 ) Europium oxide (Eu) 0.44. 0.44 g 2 O 3 ) And 0.0057 g manganese carbonate (MnCO 3 ) Uniformly mixing and grinding to obtain mixed powder;
(2) Pouring the mixed powder into an alumina crucible, calcining 5.0. 5.0 h in a box-type high temperature furnace at 1500 ℃, cooling to room temperature, and fully grinding to obtain La 0.75 Gd 0.2 AlO 3 :0.05Eu 3+ ,0.001Mn 4+ Red fluorescent powder.
The fluorescent powder prepared in example 2 of the present invention has an X-ray powder diffraction pattern shown in fig. 1, an excitation spectrum (monitor wavelength: 619 nm) shown in fig. 2, an excitation spectrum (monitor wavelength: 720 nm) shown in fig. 3, an emission spectrum (excitation wavelength: 329 nm) shown in fig. 4, and an emission spectrum (excitation wavelength: 373 nm) shown in fig. 5.
As shown in fig. 6, under the excitation of 329 and nm ultraviolet light (B wave band), the red light emission spectrum generated by the fluorescent powder is highly matched with the red area absorption spectrum of plant chlorophyll B, so that photosynthesis can be promoted; under the excitation of 373 nm ultraviolet light (A wave band), the far-infrared light emission spectrum generated by the fluorescent powder and the plant photosensitive pigment P FR Absorption spectra are highly matched due to P FR And P R Pigments can be mutually converted, so that far-red irradiation will promote P FR Pigment orientation P R Pigment conversion can effectively promote photosynthesis and fruit coloring.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; while the invention has been described in detail with reference to the foregoing embodiments, it will be appreciated by those skilled in the art that variations may be made in the techniques described in the foregoing embodiments, or equivalents may be substituted for in part or in whole; such modifications and substitutions do not depart from the spirit of the invention.
Claims (4)
1. The red fluorescent powder is characterized by comprising the following components:
RE 1-b Al 1- a-c Ga a O 3 ： b Eu 3+ , c Mn 4+
wherein, RE is La or RE is La and Gd; a is more than or equal to 0.2 and less than or equal to 0.3; b is more than or equal to 0.04 and less than or equal to 0.08, and c is more than or equal to 0.0001 and less than or equal to 0.001.
2. The red phosphor of claim 1, wherein the red phosphor emits red light with a main peak at 619 nm narrow band under ultraviolet excitation at a wavelength of about 329 nm and emits far red light with a main peak at 720 nm broad band under excitation at 373 nm.
3. A method for preparing the red fluorescent powder according to any one of claims 1 to 2, comprising the steps of:
lanthanum oxide, aluminum hydroxide, gallium oxide, europium oxide and manganese carbonate are taken as raw materials to be uniformly mixed and ground to obtain mixed powder;
calcining the mixed powder in an alumina crucible in an air atmosphere to obtain the red fluorescent powder;
wherein the temperature of the calcination is 1400-1600 ℃, and the time of the calcination is 4.0-7.0 h.
4. The use of the red phosphor according to any one of claims 1 to 2 or the red phosphor obtained by the production method according to claim 3, characterized in that the red phosphor is added to a resin as a raw material, and a plastic film or laminated glass having a property of converting ultraviolet light of two wavelength ranges into red light and far-red light is produced, and the emission spectra thereof are respectively similar to those of chlorophyll b and P plants FR The absorption spectrum of the pigment is overlapped, and the pigment is applied to the field of agriculture to promote the growth of plants.
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| CN111662714A (en) * | 2020-06-08 | 2020-09-15 | 苏州麦茂思传感技术有限公司 | Red fluorescent powder with uniform particles and preparation method thereof |
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| CN111662714A (en) * | 2020-06-08 | 2020-09-15 | 苏州麦茂思传感技术有限公司 | Red fluorescent powder with uniform particles and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Study on preparation and luminescent properties of Eu3+-doped LaAlO3 and GdAlO3;Xiaorui Dong et al.;Materials Research Bulletin;第47卷;第212-216页 * |
| Zero-thermal-quenching of Mn4+ far-red-emitting in LaAlO3 perovskite phosphor via energy compensation of electrons’ traps;Shuangqiang Fang et al.;Chemical Engineering Journal;第389卷;第124297页 * |
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