CN113861979B - Mn (manganese) 4+ Activated antimonate red fluorescent powder and preparation method and application thereof - Google Patents

Mn (manganese) 4+ Activated antimonate red fluorescent powder and preparation method and application thereof Download PDF

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CN113861979B
CN113861979B CN202111248363.3A CN202111248363A CN113861979B CN 113861979 B CN113861979 B CN 113861979B CN 202111248363 A CN202111248363 A CN 202111248363A CN 113861979 B CN113861979 B CN 113861979B
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fluorescent powder
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CN113861979A (en
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郭锐
李志远
罗岚
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Nanchang University
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    • 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
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    • 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
    • A01G9/00—Cultivation in receptacles, forcing-frames or greenhouses; Edging for beds, lawn or the like
    • A01G9/20—Forcing-frames; Lights, i.e. glass panels covering the forcing-frames

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Abstract

The invention discloses Mn & lt 4+ & gt activated antimonite red fluorescent powder and a preparation method and application thereof. The chemical general formula of the fluorescent powderIs Ca 3‑6y LiSb 1‑x O 6 :xMn 4+ ,3yNa + ,3yLn 3+ (ii) a Wherein x is more than 0 and less than or equal to 0.03, Y is more than or equal to 0 and less than or equal to 0.1, ln is any one or more of Lu, Y, gd and La. The fluorescent powder can be effectively excited by ultraviolet light and blue light to emit red fluorescent light within the wavelength range of 625-800 nanometers. The invention also provides a preparation method of the material, which is prepared by adopting a high-temperature solid-phase synthesis method, has simple synthesis process and low production cost, and is easy for industrial production. The fluorescent powder can be widely applied to LED plant growth lamps excited by near ultraviolet or blue light chips, and can also be used as compensation red powder for low-color-temperature high-color-rendering-index white-light LED lamps.

Description

Mn (manganese) 4+ Activated antimonate red fluorescent powder and preparation method and application thereof
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to Mn & lt 4+ & gt activated antimonite red fluorescent powder as well as a preparation method and application thereof.
Background
The light is an essential environmental factor for plant growth and development. In order to solve the problem of insufficient plant illumination caused by factors such as severe weather and environmental pollution, various artificial light sources applied to plant illumination are produced. Conventional artificial light sources mainly include incandescent lamps, halogen lamps, high-pressure sodium lamps, fluorescent lamps, and the like. Since the light sources are designed for white light illumination based on human vision, the white light illumination is not matched with the growth requirements of plants, and the white light illumination has short service life and high energy consumption. The LED plant growth lamp shows great development potential in the plant lighting industry due to the advantages of controllable spectrum, small volume, low heat productivity, long service life and the like.
Research shows that plants do not absorb all light simultaneously, but absorb light in a specific wave band, and the absorption spectrum of different green plants to light is basically the same. The chlorophyll and carotenoid of plants participating in photosynthesis have the strongest light absorption at 430-450 nm, while the chlorophyll has the second obvious absorption band at 640-660 nm, which shows that the photosynthesis spectrum is mainly concentrated in the blue light region and the deep red light region. In addition, the phytochrome includes 660 nm red light absorption type P R And a far-red light absorption type P of 730 nm FR Has important function for regulating and controlling the photomorphogenetic process of plant growth, development, differentiation and the like. Currently, absorption spectra, blue and deep red fluorescence are directed at plant growthThe powder has been widely studied, but the research on the far-red phosphor is relatively insufficient.
Mn of non-rare earths 4+ Ion due to its unique 3d 3 Electronic structures, doped phosphors of which generally exhibit broadband absorption and narrow-band red emission characteristics. At present, mn 4+ The doped fluorescent powder mainly comprises two main categories of fluoride and oxysalt. Due to Mn in the oxysalt 4+ -O 2- Covalent ratio of Mn in fluoride 4+ -F - Strong, mn in oxysalts 4+ The emission wavelength is longer and deviates from the sensitive area of the human eye. Mn 4+ The doped oxide fluorescent powder is more beneficial to realizing far-red light emission and can effectively cover a far-red light region absorbed by plant pigments. Therefore, novel Mn which is excellent in development property and easy and convenient to prepare is developed 4+ The doped far-red fluorescent powder has important significance for the application of the LED plant growth lamp.
Disclosure of Invention
The LED plant growth lamp aims to overcome the defects and shortcomings in the prior art and solve the bottleneck problem of red light components in the existing LED plant growth lamp. The invention provides Mn & lt 4+ & gt activated antimonite red fluorescent powder capable of emitting red fluorescence when excited by excitation light sources such as near ultraviolet light or blue light and the like, and a preparation method and application thereof.
Mn4+ activated antimonate red phosphor, wherein the chemical general formula of the phosphor is Ca 3-6y LiSb 1-x O 6 :xMn 4+ ,3yNa + ,3yLn 3+ ；
Wherein x is more than 0 and less than or equal to 0.03, Y is more than or equal to 0 and less than or equal to 0.1, ln is any one or more of Lu, Y, gd and La.
Furthermore, x and y are preferably in the range of 0.001 to 0.01 and 0 to 0.05.
A preparation method of Mn & lt 4+ & gt activated antimonite red fluorescent powder comprises the following steps:
1) According to the chemical formula Ca 3-6y LiSb 1-x O 6 :xMn 4+ ,3yNa + ,3yLn 3+ The stoichiometric ratio of each element in the composition is respectively weighing Ca-containing compound, li-containing compound and Sb-containing compoundPreparing a compound, a Mn-containing compound, a Na-containing compound and an Ln-containing compound for later use;
2) Mixing the compound weighed in the step 1) with an ethanol solution, and fully grinding to obtain a precursor;
3) Heating and calcining the precursor obtained in the step 2) in an air atmosphere, naturally cooling to room temperature after the reaction is finished, taking out, and grinding to be uniform again to obtain the red fluorescent powder.
Further, the Ca-containing compound in step 1) is one or more of calcium oxide, calcium carbonate and calcium hydroxide.
Further, the compound containing Li in the step 1) is one or more of lithium oxide, lithium carbonate and lithium hydroxide.
Further, the compound containing Sb in the step 1) is one or two of antimony pentoxide and antimony trioxide.
Further, the Mn-containing compound in the step 1) is one or more of manganese carbonate, manganese nitrate, manganese acetate, manganese oxalate and manganese dioxide.
Further, the Na-containing compound in the step 1) is one or more of sodium oxide, sodium carbonate, sodium hydroxide and sodium bicarbonate; the Ln-containing compound is one or more of lutetium oxide, yttrium oxide, gadolinium oxide and lanthanum oxide.
Further, the grinding time in the step 2) is 0.5-1 hour.
Further, the calcining temperature in the step 3) is 800-1100 ℃, and the time is 3-12 hours; more preferably at 850-950 ℃ for 4-8 hours.
Further, the fluorescent powder of the invention emits red fluorescence with the dominant wavelength of about 694 nanometers under the excitation of near ultraviolet to blue light with the wavelength of 250-550 nanometers.
The Mn & lt 4+ & gt activated antimonite red fluorescent powder prepared by the technical scheme of the invention is applied to preparing an LED plant growth lamp excited by a near ultraviolet or blue light chip.
Compared with the prior art, the invention has the beneficial effects that:
1. the excitation wavelength of the fluorescent powder is in a near ultraviolet to blue light region of 250-550 nanometers, and the fluorescent powder can be well matched with a commercial near ultraviolet or blue light LED chip.
2. The fluorescent powder can emit red fluorescence with the dominant wavelength of about 694 nanometers under the excitation of near ultraviolet or blue light, and can be effectively absorbed by plant pigment.
3. The fluorescent powder provided by the invention has the advantages of simple preparation process, low synthesis temperature, no pollution and easiness in mass production, and can be widely applied to LED plant growth lamps excited by near ultraviolet or blue light chips.
Drawings
FIG. 1 shows Mn prepared in examples 4 to 7 of the present invention 4+ And (3) an X-ray diffraction spectrum of the doped red fluorescent powder.
FIG. 2 shows Mn prepared in examples 4 to 7 of the present invention 4+ Excitation spectrum of doped red phosphor.
FIG. 3 shows Mn prepared in examples 4 to 7 of the present invention 4+ And the emission spectrum of the doped red fluorescent powder.
FIG. 4 shows Mn prepared in example 4 of the present invention 4+ Scanning electron microscope photo of doped red fluorescent powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments. The examples, in which specific conditions are not specified, were conducted under 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.
Example 1
According to Ca 3 LiSb 0.998 O 6 :0.2％Mn 4+ Accurately weighing the following raw materials in a stoichiometric ratio: 3.0027 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6144 grams antimony pentoxide, and 0.0023 grams manganese carbonate. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 850 ℃ under the air atmosphere for calcination for 8 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain the productTo a Mn 4+ Activated antimonate red phosphor.
Example 2
According to Ca 3 LiSb 0.994 O 6 :0.6％Mn 4+ Accurately weighing the following raw materials in a stoichiometric ratio of: 3.0027 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6079 grams antimony pentoxide, and 0.0069 grams manganese carbonate. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 900 ℃ in air atmosphere for calcination for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn 4+ Activated antimonate red phosphor.
Example 3
According to Ca 3 LiSb 0.988 O 6 :1.2％Mn 4+ Accurately weighing the following raw materials in a stoichiometric ratio: 3.0027 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.5982 grams antimony pentoxide, and 0.0138 grams manganese carbonate. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 950 ℃ in air atmosphere for calcination for 4 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn 4+ Activated antimonate red phosphor.
Example 4
According to Ca 2.82 LiSb 0.994 O 6 :0.6％Mn 4+ ,9％Na + ,9％Lu 3+ Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 grams of calcium carbonate, 0.3695 grams of lithium carbonate, 1.6079 grams of antimony pentoxide, 0.0069 grams of manganese carbonate, 0.0477 grams of sodium carbonate, and 0.1791 grams of lutetium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 900 ℃ in air atmosphere for calcination for 6 hours. After the calcined and sintered product is naturally cooled to room temperature, the calcined and sintered product is taken out and ground again uniformly to obtain Mn 4+ Activated antimonate red phosphor.
FIG. 4 is a SEM photograph of a sample prepared in this example, and it can be seen that the prepared sample has an irregular block structure, the particle size is in the micron level, and the surface of the sample is relatively smooth, indicating that the crystallinity is good.
Example 5
According to Ca 2.82 LiSb 0.994 O 6 :0.6％Mn 4+ ,9％Na + ,9％Y 3+ Accurately weighing the following raw materials in a stoichiometric ratio of: 2.8225 g calcium carbonate, 0.3695 g lithium carbonate, 1.6079 g antimony pentoxide, 0.0069 g manganese carbonate, 0.0477 g sodium carbonate and 0.1016 g yttrium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 900 ℃ in air atmosphere for calcination for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn 4+ Activated antimonate red phosphor.
Example 6
According to Ca 2.82 LiSb 0.994 O 6 :0.6％Mn 4+ ,9％Na + ,9％Gd 3+ Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 g calcium carbonate, 0.3695 g lithium carbonate, 1.6079 g antimony pentoxide, 0.0069 g manganese carbonate, 0.0477 g sodium carbonate and 0.1631 g gadolinium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be calcined for 6 hours at the temperature of 900 ℃ under the air atmosphere. After the calcined and sintered product is naturally cooled to room temperature, the calcined and sintered product is taken out and ground again uniformly to obtain Mn 4+ Activated antimonate red phosphor.
Example 7
According to Ca 2.82 LiSb 0.994 O 6 :0.6％Mn 4+ ,9％Na + ,9％La 3+ Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 g calcium carbonate, 0.3695 g lithium carbonate, 1.6079 g antimony pentoxide, 0.0069 g manganese carbonate, 0.0477 g sodium carbonate and 0.1466 g lanthanum oxide. Fully and uniformly grinding the raw materials and a proper amount of ethanol solution in an agate mortar, putting the obtained mixture into a muffle furnace, heating to 900 ℃ in air atmosphere, and calciningAnd burning for 6 hours. After the calcined and sintered product is naturally cooled to room temperature, the calcined and sintered product is taken out and ground again uniformly to obtain Mn 4+ Activated antimonate red phosphor.
FIG. 1 is an X-ray powder diffraction pattern of samples prepared in examples 4-7, and the results of the tests show that all the samples prepared are relatively crystalline and are single-phase materials.
FIGS. 2 and 3 are the excitation spectrum and the emission spectrum of the samples obtained in examples 4 to 7, respectively, the excitation spectrum range of the samples is 250 to 550 nm, the emission spectrum range is 625 to 800 nm, and the main emission peak is located at more than 694 nm.
Example 8
According to Ca 2.94 LiSb 0.994 O 6 :0.6％Mn 4+ ,3％Na + ,3％Lu 3+ Accurately weighing the following raw materials in a stoichiometric ratio: 2.9426 grams of calcium carbonate, 0.3695 grams of lithium carbonate, 1.6079 grams of antimony pentoxide, 0.0069 grams of manganese carbonate, 0.0159 grams of sodium carbonate, and 0.0597 grams of lutetium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 900 ℃ in air atmosphere for calcination for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn 4+ Activated antimonate red phosphor.
Example 9
According to Ca 2.88 LiSb 0.994 O 6 :0.6％Mn 4+ ,6％Na + ,6％Y 3+ Accurately weighing the following raw materials in a stoichiometric ratio of: 2.8826 grams of calcium carbonate, 0.3695 grams of lithium carbonate, 1.6079 grams of antimony pentoxide, 0.0069 grams of manganese carbonate, 0.0318 grams of sodium carbonate, and 0.0677 grams of yttrium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be calcined for 6 hours at the temperature of 900 ℃ under the air atmosphere. After the calcined and sintered product is naturally cooled to room temperature, the calcined and sintered product is taken out and ground again uniformly to obtain Mn 4+ Activated antimonate red phosphor.
Example 10
According to Ca 2.76 LiSb 0.994 O 6 :0.6％Mn 4+ ,12％Na + ,12％Gd 3+ Accurately weighing the following raw materials in a stoichiometric ratio: 2.7625 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6079 grams antimony pentoxide, 0.0069 grams manganese carbonate, 0.0636 grams sodium carbonate, and 0.2175 grams gadolinium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be calcined for 6 hours at the temperature of 900 ℃ under the air atmosphere. After the calcined and sintered product is naturally cooled to room temperature, the calcined and sintered product is taken out and ground again uniformly to obtain Mn 4+ Activated antimonate red phosphor.
Example 11
According to Ca 2.7 LiSb 0.994 O 6 :0.6％Mn 4+ ,15％Na + ,15％La 3+ Accurately weighing the following raw materials in a stoichiometric ratio of: 2.7024 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6079 grams antimony pentoxide, 0.0069 grams manganese carbonate, 0.0795 grams sodium carbonate, and 0.2444 grams lanthanum oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 900 ℃ in air atmosphere for calcination for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn 4+ Activated antimonate red phosphor.
Example 12
According to Ca 2.82 LiSb 0.988 O 6 :1.2％Mn 4+ ,9％Na + ,9％Lu 3+ Accurately weighing the following raw materials in a stoichiometric ratio of: 2.8225 grams of calcium carbonate, 0.3695 grams of lithium carbonate, 1.5982 grams of antimony pentoxide, 0.0138 grams of manganese carbonate, 0.0477 grams of sodium carbonate, and 0.1791 grams of lutetium oxide. The raw materials and a proper amount of ethanol solution are fully and uniformly ground in an agate mortar, and the obtained mixture is put into a muffle furnace to be heated to 900 ℃ in air atmosphere for calcination for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn 4+ Activated antimonate red phosphor.
The above-described embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention, and any such changes, substitutions, improvements and the like are intended to be included within the scope of the invention.

Claims (10)

1. Mn (manganese) 4+ The activated antimonate red phosphor is characterized in that the chemical general formula of the phosphor is Ca 3- 6y LiSb 1-x O 6 :xMn 4+ ,3yNa + ,3yLn 3+ ；
Wherein x is more than 0 and less than or equal to 0.03, Y is more than 0 and less than or equal to 0.1, ln is any one of Lu, Y, gd and La.
2. A Mn as claimed in claim 1 4+ The activated antimonate red fluorescent powder is characterized in that x and y are in the range of 0.001-0.01 and 0-0.05 respectively.
3. An Mn as claimed in claim 1 or 2 4+ The preparation method of the activated antimonate red fluorescent powder is characterized by comprising the following steps:
1) According to the chemical formula Ca 3-6y LiSb 1-x O 6 :xMn 4+ ,3yNa + ,3yLn 3+ Respectively weighing Ca-containing compound, li-containing compound, sb-containing compound, mn-containing compound, na-containing compound and Ln-containing compound for later use according to the stoichiometric ratio of each element;
2) Mixing the compound weighed in the step 1) with an ethanol solution, and fully grinding to obtain a precursor;
3) Heating and calcining the precursor obtained in the step 2) in an air atmosphere, naturally cooling to room temperature after the reaction is finished, taking out, and grinding to be uniform again to obtain the red fluorescent powder.
4. A Mn according to claim 3 4+ The preparation method of the activated antimonate red phosphor is characterized in that the Ca-containing compound in the step 1)The substance is one or more of calcium oxide, calcium carbonate and calcium hydroxide.
5. An Mn as set forth in claim 3 4+ The preparation method of the activated antimonate red fluorescent powder is characterized in that the compound containing Li in the step 1) is one or more of lithium oxide, lithium carbonate and lithium hydroxide.
6. An Mn as set forth in claim 3 4+ The preparation method of the activated antimonate red fluorescent powder is characterized in that the Sb-containing compound in the step 1) is one or two of antimony pentoxide and antimony trioxide.
7. An Mn as set forth in claim 3 4+ The preparation method of the activated antimonate red fluorescent powder is characterized in that the Mn-containing compound in the step 1) is one or more of manganese carbonate, manganese nitrate, manganese acetate, manganese oxalate and manganese dioxide.
8. An Mn as set forth in claim 3 4+ The preparation method of the activated antimonate red fluorescent powder is characterized in that the compound containing Na in the step 1) is one or more of sodium oxide, sodium carbonate, sodium hydroxide and sodium bicarbonate; the Ln-containing compound is one of lutetium oxide, yttrium oxide, gadolinium oxide and lanthanum oxide.
9. A Mn according to claim 3 4+ The preparation method of the activated antimonate red fluorescent powder is characterized in that the calcining temperature in the step 3) is 800-1100 ℃ and the time is 3-12 hours.
10. An Mn as set forth in any of claims 1 to 2 4+ The activated antimonate red fluorescent powder is applied to preparing an LED plant growth lamp excited by a near ultraviolet or blue light chip.
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