CN113861979A - 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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CN113861979A
CN113861979A CN202111248363.3A CN202111248363A CN113861979A CN 113861979 A CN113861979 A CN 113861979A CN 202111248363 A CN202111248363 A CN 202111248363A CN 113861979 A CN113861979 A CN 113861979A
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containing compound
red phosphor
oxide
manganese
antimonate
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CN113861979B (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
    • C09K11/7714—Antimonates; Arsenates
    • 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 Mn4+ -activated antimonate red fluorescent powder and a preparation method and application thereof. The chemical general formula of the fluorescent powder is Ca3‑6yLiSb1‑xO6:xMn4+,3yNa+,3yLn3+(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, and 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 Mn4+ -activated antimonate 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 the carotenoid of the plants participating in the photosynthesis have the strongest light absorption at the 450 nm of 430-450 nm, and the chlorophyll has a second obvious absorption band at the 660 nm of 640-660 nm, which indicates that the photosynthesis spectrum is mainly concentrated in the blue light region and the deep red light region. In addition, the photosensitizing pigment includes a red light absorption type P of 660 nmRAnd a far-red light absorption type P of 730 nmFRHas important function for regulating and controlling the photomorphogenetic process of plant growth, development, differentiation and the like. At present, blue and deep red phosphors have been widely studied for the absorption spectrum of plant growth, but the research on far-red phosphors is relatively insufficient.
Mn of non-rare earths4+Ion due to its unique 3d3Electronic structures, doped phosphors of which generally exhibit broadband absorption and narrow-band red emission characteristics. At present, Mn4+The doped fluorescent powder mainly comprises two main types of fluoride and oxysalt. Due to Mn in the oxysalt4+-O2-Covalent ratio of Mn in fluoride4+-F-Strong, Mn in oxysalts4+The emission wavelength is longer and deviates from the sensitive area of the human eye. Mn4+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 developed4+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 Mn4+ activated antimonate 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 powder, wherein the chemical general formula of the phosphor powder is Ca3-6yLiSb1-xO6:xMn4+,3yNa+,3yLn3+；
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, and Ln is any one or more of Lu, Y, Gd and La.
Further, x and y are preferably in the range of 0.001 to 0.01 and 0 to 0.05.
A preparation method of Mn4+ activated antimonate red phosphor comprises the following steps:
1) according to the chemical formula Ca3-6yLiSb1-xO6:xMn4+,3yNa+,3yLn3+Respectively weighing Ca-containing compound, Li-containing compound, Sb-containing compound, Mn-containing compound, Na-containing compound and Ln-containing compound according to the stoichiometric ratio of the elements;
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 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 850 ℃ and 950 ℃ for 4 to 8 hours.
Further, the phosphor of the present invention emits red fluorescence with a dominant wavelength of about 694 nm under the excitation of near ultraviolet to blue light with a wavelength of 250-550 nm.
The Mn4+ -activated antimonate 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 the near ultraviolet to blue light region of 250-550 nm, 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 invention4+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 invention4+Excitation spectrum of doped red phosphor.
FIG. 3 shows Mn prepared in examples 4 to 7 of the present invention4+And the emission spectrum of the doped red fluorescent powder.
FIG. 4Mn prepared for inventive example 44+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 Ca3LiSb0.998O6:0.2％Mn4+Accurately weighing the following raw materials in a stoichiometric ratio: 3.0027 g of calcium carbonate, 0.3695 g of lithium carbonate, 1.6144 g of antimony pentoxide and 0.0023 g of 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 Mn4+Activated antimonate red phosphor.
Example 2
According to Ca3LiSb0.994O6:0.6％Mn4+Accurately weighing the following raw materials in a stoichiometric ratio: 3.0027 g of calcium carbonate, 0.3695 g of lithium carbonate, 1.6079 g of antimony pentoxide and 0.0069 g of 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 Mn4+Activated antimonate red phosphor.
Example 3
According to Ca3LiSb0.988O6:1.2％Mn4+Accurately weighing the following raw materials in a stoichiometric ratio: 3.0027 g of calcium carbonate, 0.3695 g of lithium carbonate, 1.5982 g of antimony pentoxide and 0.0138 g of manganese carbonate. Mixing the raw materials with proper amount of BAfter the alcoholic solution is fully and uniformly ground in an agate mortar, the obtained mixture is put into a muffle furnace and is heated to 950 ℃ under the air atmosphere for calcining for 4 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn4+Activated antimonate red phosphor.
Example 4
According to Ca2.82LiSb0.994O6:0.6％Mn4+,9％Na+,9％Lu3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6079 grams antimony pentoxide, 0.0069 grams manganese carbonate, 0.0477 grams sodium carbonate, and 0.1791 grams 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 Mn4+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 Ca2.82LiSb0.994O6:0.6％Mn4+,9％Na+,9％Y3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6079 grams antimony pentoxide, 0.0069 grams manganese carbonate, 0.0477 grams sodium carbonate, and 0.1016 grams 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 Mn4+Activated antimonate red phosphor.
Example 6
According to Ca2.82LiSb0.994O6:0.6％Mn4+,9％Na+,9％Gd3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 g of calcium carbonate, 0.3695 g of lithium carbonate, 1.6079 g of antimony pentoxide, 0.0069 g of manganese carbonate, 0.0477 g of sodium carbonate and 0.1631 g of 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 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 Mn4+Activated antimonate red phosphor.
Example 7
According to Ca2.82LiSb0.994O6:0.6％Mn4+,9％Na+,9％La3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.6079 grams antimony pentoxide, 0.0069 grams manganese carbonate, 0.0477 grams sodium carbonate, and 0.1466 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 Mn4+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 4-7, respectively, wherein the excitation spectrum range of the sample is 250-550 nm, the emission spectrum range is 625-800 nm, and the main emission peak is located at more than 694 nm.
Example 8
According to Ca2.94LiSb0.994O6:0.6％Mn4+,3％Na+,3％Lu3+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. Mixing the raw materials with appropriate amount of ethanol solutionAfter fully and uniformly grinding in an agate mortar, putting the obtained mixture into a muffle furnace, and heating to 900 ℃ in an air atmosphere to calcine for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn4+Activated antimonate red phosphor.
Example 9
According to Ca2.88LiSb0.994O6:0.6％Mn4+,6％Na+,6％Y3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.8826 g of calcium carbonate, 0.3695 g of lithium carbonate, 1.6079 g of antimony pentoxide, 0.0069 g of manganese carbonate, 0.0318 g of sodium carbonate and 0.0677 g 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 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 Mn4+Activated antimonate red phosphor.
Example 10
According to Ca2.76LiSb0.994O6:0.6％Mn4+,12％Na+,12％Gd3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.7625 grams of calcium carbonate, 0.3695 grams of lithium carbonate, 1.6079 grams of antimony pentoxide, 0.0069 grams of manganese carbonate, 0.0636 grams of sodium carbonate, and 0.2175 grams of 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 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 Mn4+Activated antimonate red phosphor.
Example 11
According to Ca2.7LiSb0.994O6:0.6％Mn4+,15％Na+,15％La3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.7024 g of calcium carbonate, 0.3695 g of lithium carbonate, 1.6079 g of antimony pentoxide, 0.0069 g of manganese carbonate, 0.0795 g of sodium carbonate and 0.2444 g of lanthanum oxide. Mixing the raw materials with appropriate amountAfter the ethanol solution is fully and uniformly ground in an agate mortar, the obtained mixture is put into a muffle furnace and is heated to 900 ℃ under the air atmosphere for calcination for 6 hours. After calcining and sintering, naturally cooling to room temperature, taking out and grinding uniformly again to obtain Mn4+Activated antimonate red phosphor.
Example 12
According to Ca2.82LiSb0.988O6:1.2％Mn4+,9％Na+,9％Lu3+Accurately weighing the following raw materials in a stoichiometric ratio: 2.8225 grams calcium carbonate, 0.3695 grams lithium carbonate, 1.5982 grams antimony pentoxide, 0.0138 grams manganese carbonate, 0.0477 grams sodium carbonate, and 0.1791 grams 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 Mn4+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 can be made by one skilled in the art, and any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The Mn4+ -activated antimonate red phosphor is characterized in that the chemical general formula of the phosphor is Ca3- 6yLiSb1-xO6:xMn4+,3yNa+,3yLn3+；
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, and Ln is any one or more of Lu, Y, Gd and La.
2. The Mn4+ -activated antimonate red phosphor of claim 1, wherein x and y are in the range of 0.001 < x.ltoreq.0.01, and 0. ltoreq.y.ltoreq.0.05.
3. The method of claim 1 or 2, wherein the method comprises the steps of:
1) according to the chemical formula Ca3-6yLiSb1-xO6:xMn4+,3yNa+,3yLn3+Respectively weighing Ca-containing compound, Li-containing compound, Sb-containing compound, Mn-containing compound, Na-containing compound and Ln-containing compound according to the stoichiometric ratio of the elements;
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. The method for preparing Mn4+ -activated antimonate red phosphor according to claim 3, wherein the Ca-containing compound in step 1) is one or more of calcium oxide, calcium carbonate and calcium hydroxide.
5. The method for preparing Mn4+ -activated antimonate red phosphor according to claim 3, wherein the Li-containing compound in step 1) is one or more of lithium oxide, lithium carbonate and lithium hydroxide.
6. The method for preparing Mn4+ -activated antimonate red phosphor according to claim 3, wherein the Sb-containing compound in step 1) is one or two of antimony pentoxide and antimony trioxide.
7. The method for preparing Mn4+ -activated antimonate red phosphor according to claim 3, wherein the Mn-containing compound in step 1) is one or more of manganese carbonate, manganese nitrate, manganese acetate, manganese oxalate and manganese dioxide.
8. The method for preparing Mn4+ -activated antimonate red phosphor according to claim 3, wherein the Na-containing compound in 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.
9. The method as claimed in claim 3, wherein the calcining temperature in step 3) is 800-1100 ℃ for 3-12 hours.
10. An application of the Mn4+ -activated antimonate red phosphor as claimed in any one of claims 1 to 9 in preparation of a near ultraviolet or blue light chip excited LED plant growth lamp.
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