CN110862821B - Phosphate-based fluorescent powder material and preparation method and application thereof - Google Patents
Phosphate-based fluorescent powder material and preparation method and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 87
- 239000000463 material Substances 0.000 title claims abstract description 79
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 53
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 49
- 239000010452 phosphate Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 238000000227 grinding Methods 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 12
- 238000010304 firing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 51
- 239000000047 product Substances 0.000 claims description 27
- 238000007873 sieving Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 229910017677 NH4H2 Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims 1
- 239000012856 weighed raw material Substances 0.000 abstract description 10
- 238000010923 batch production Methods 0.000 abstract description 4
- 238000000295 emission spectrum Methods 0.000 description 15
- 238000000695 excitation spectrum Methods 0.000 description 15
- 230000005284 excitation Effects 0.000 description 14
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 7
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 2
- 229910010199 LiAl Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 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
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
- C09K11/701—Chalcogenides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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Abstract
The invention discloses a phosphate-based fluorescent powder material, a preparation method and application thereof, and the preparation method and application of the fluorescent powder materialThe chemical expression is AB1‑xP2O7xCr, wherein A is at least one of Li, Na and K, and x is more than or equal to 0.01 and less than or equal to 0.1; the preparation method comprises the following steps: 1) accurately weighing the raw materials according to the chemical dose ratio of the phosphate-based fluorescent powder material; 2) fully and uniformly mixing the weighed raw materials, and firing the mixture at a high temperature in an air atmosphere to obtain a firing product; 3) and grinding the burning product into powder, and then washing and drying to obtain the phosphate-based fluorescent powder material. The fluorescent powder material can be effectively excited by a blue light LED chip and emits 750-1100 nm broadband near-infrared light, and is good in chemical stability, excellent in luminous performance, simple in preparation method, convenient to operate, low in cost, free of pollution and suitable for industrial batch production.
Description
Technical Field
The invention relates to a phosphate-based fluorescent powder material and a preparation method and application thereof, belonging to the technical field of solid luminescent materials.
Background
The near-infrared light source has wide application in the fields of food detection, minimally invasive diagnosis, biological imaging, solar cell, spectrum test and the like. The current commercial near-infrared light sources mainly comprise tungsten filament incandescent lamps, near-infrared lasers and near-infrared LEDs. The tungsten filament incandescent lamp can provide an ultra-wide continuous light source from visible light to near infrared light, but has short service life, large volume, high working temperature and low luminous efficiency of the near infrared light part; the near-infrared laser and the near-infrared LED have high luminous intensity, but have the intrinsic characteristic of narrow coverage of an emission band. For applications requiring miniaturized and broadband-emitting near-infrared light sources, these light sources are not ideal, and there is a strong need to construct a long-life, small-volume, high-efficiency, wide-spectrum near-infrared light source from a new approach.
The LED device excited by the blue light chip is rapidly developed in the field of illumination, and becomes a latest generation of illumination light source, which provides a new way and thought for the research and development of broadband near-infrared light sources. The novel fluorescence conversion type broadband near-infrared LED light source can be built by compounding the near-infrared fluorescent powder and the blue light LED chip. Due to the mature preparation process and excellent performance of the blue light LED chip, the novel broadband near-infrared light source has the advantages of low cost, good thermal stability, high power, energy conservation and environmental protection. On the other hand, the corresponding fluorescent powder material is prepared by selecting a proper matrix material and luminous ion combination, and can provide continuously adjustable broadband near-infrared light emission under the excitation of a blue light chip.
At present, the research on the fluorescent powder material is mainly focused on a visible light region, the research on the fluorescent powder material which can be effectively excited by a blue light chip and can emit broadband near infrared light is less, and no corresponding mature product is provided in each field. Therefore, further intensive research on near-infrared fluorescent powder materials is needed, and a broadband near-infrared light source with high performance and multiple purposes is constructed in a new way.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a phosphate-based fluorescent powder material, a preparation method and application thereof, wherein the material is stable in chemical property and excellent in luminous performance, can be effectively excited by visible light in the ranges of 400-520 nm and 550-780 nm, and emits broadband near-infrared light in the range of 750-1100 nm; the preparation method of the material is simple, convenient to operate, low in cost, free of pollution and suitable for industrial batch production.
The technical scheme is as follows: the invention provides a phosphate-based fluorescent powder material, and the chemical expression of the fluorescent powder material is AB1-xP2O7xCr, wherein A is at least one of Li, Na and K, and x is more than or equal to 0.01 and less than or equal to 0.1.
Wherein:
the chemical expression of the fluorescent powder material can also be AB1-x-yP2O7xCr, yYb, wherein A is at least one of Li, Na and K, B is at least one of Al, Ga, In and Sc, x is more than or equal to 0.01 and less than or equal to 0.1, and y is more than 0 and less than or equal to 0.05.
The fluorescent powder material can be excited by visible light in the range of 400-520 nm and 550-780 nm and emits broadband near infrared light in the range of 750-1100 nm.
The invention also provides a preparation method of the phosphate-based fluorescent powder material, which adopts a high-temperature solid phase method for preparation, and the method comprises the following steps:
1) accurately weighing carbonate of Li, Na and K, oxide of Al, Ga, In and Sc and NH according to the chemical dose ratio of the phosphate-based fluorescent powder material4H2PO4As a raw material;
2) fully and uniformly mixing the raw materials weighed in the step 1) to obtain a mixture, and firing the mixture at a high temperature in an air atmosphere to obtain a firing product;
3) grinding the burning product obtained in the step 2) into powder, and then washing and drying to obtain the phosphate-based fluorescent powder material.
Wherein:
the excess percentage of the Li carbonate in the step 1) is 0-15%, and NH4H2PO4The excess percentage is 0-10%.
The high-temperature burning condition in the step 2) is as follows: the temperature is 800-1100 ℃, the burning time is 2-10 h, and the burning times are at least 1 time.
Grinding the burning product into powder in the step 3), and then washing and drying, namely grinding the burning product into powder, sieving the powder with a 200-mesh sieve, washing for 1-3 times, centrifuging and drying the precipitate at the temperature of 60-80 ℃.
The invention also provides an application of the phosphate-based fluorescent powder material, and the phosphate-based fluorescent powder material is applied to construction of a broadband near-infrared fluorescence conversion type LED device.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the invention provides a novel fluorescent powder material type, which is wide in excitation range, can be excited by visible light in the ranges of 400-520 nm and 550-780 nm, can emit broadband near infrared light in the range of 750-1100 nm, has the emission wavelength completely in a near infrared band, and is large in half-peak width, high in luminous efficiency and good in luminous heat stability; the fluorescent powder material can be packaged with a blue light or red light LED chip to construct a broadband near-infrared fluorescence conversion type LED device, can be used as a novel near-infrared light source, and has the technical advantages of high energy efficiency, small size, wide spectrum and the like.
2. The fluorescent powder material prepared by the invention has stable property, and the luminous intensity is basically unchanged through the processes of heating, water soaking and the like.
3. The invention also provides a preparation method of the fluorescent powder material, the fluorescent powder material is synthesized by adopting a solid-phase reaction method, and the method is simple, convenient to operate, low in cost, free of pollution and suitable for industrial batch production.
Drawings
FIG. 1 is a graph showing excitation and emission spectra of a phosphate-based phosphor material of example 1 of the present invention, with a monitoring wavelength of 835nm and an excitation wavelength of 450 nm;
FIG. 2 is a graph showing excitation and emission spectra of a phosphate-based phosphor material in example 2 of the present invention, with a monitoring wavelength of 790nm and an excitation wavelength of 450 nm;
FIG. 3 is an excitation and emission spectra of a phosphate-based phosphor material of example 3 of the present invention, with a monitoring wavelength of 870nm and an excitation wavelength of 450 nm;
FIG. 4 is a graph showing excitation and emission spectra of a phosphate-based phosphor material of example 4 of the present invention, with a monitor wavelength of 875nm and an excitation wavelength of 450 nm;
FIG. 5 is a graph showing excitation and emission spectra of a phosphate-based phosphor material of example 6, with a monitor wavelength of 875nm and an excitation wavelength of 450 nm;
FIG. 6 shows the excitation and emission spectra of the phosphor-based phosphor material of example 7 of the present invention, with a monitor wavelength of 875nm and an excitation wavelength of 450 nm.
Detailed Description
The invention provides a phosphate-based fluorescent powder material and a preparation method and application thereof, wherein the phosphate-based fluorescent powder material has a chemical expression as follows: AB1-x-yP2O7xCr, yYb, wherein A is at least one of Li, Na and K, B is at least one of Al, Ga, In and Sc, x is more than or equal to 0.01 and less than or equal to 0.1, y is more than or equal to 0 and less than or equal to 0.05, and Cr is used as a luminescent ion and is an essential component; yb plays a role in further broadening the emission wavelength of the phosphor, and is an unnecessary component, which may be selectively added or not added; no proportion requirement exists between the two; the fluorescent powder material can be effectively excited by a blue light LED chip, andthe material emits 750-1100 nm broadband near-infrared light, is good in chemical stability, excellent in light emitting performance, simple in preparation method, convenient to operate, low in cost and free of pollution, and is suitable for industrial batch production.
Example 1:
a phosphate-based phosphor material, the chemical expression of the phosphor is LiAl0.99P2O70.01Cr, and the preparation steps are as follows:
1. accurately weighing raw material Li2CO3 0.5mmol，Al2O3 0.495mmol，NH4H2PO4 2mmol，Cr2O30.005mmol；
2. Fully mixing the weighed raw materials, burning for 6 hours at 800 ℃ in air, and cooling to room temperature along with a furnace to obtain a burning product;
3. fully grinding the obtained burning product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 1 time by deionized water, and drying the powder at 60 ℃ to obtain the LiAl of the invention0.97P2O70.01Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are shown in figure 1, and it can be seen from the figure that the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-780 nm and emits broadband near-infrared light in the range of 750-1000 nm.
Example 2:
a phosphate-based phosphor material, the chemical expression of the phosphor is NaGa0.98P2O70.02Cr, and the preparation steps are as follows:
1. accurately weighing raw material Na2CO3 0.5mmol，Ga2O3 0.49mmol，NH4H2PO4 2mmol，Cr2O30.01mmol；
2. Fully mixing the weighed raw materials, burning the raw materials in air at 900 ℃ for 8 hours, and cooling the raw materials to room temperature along with a furnace to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 2 times by deionized water, and 8Drying at 0 ℃ to obtain the NaGa0.97P2O70.02Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are shown in figure 2, and it can be seen from the figure that the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-780 nm, and emits broadband near-infrared light in the range of 750-900 nm.
Example 3:
a phosphate-based phosphor material, wherein the chemical expression of the phosphor is KIn0.97P2O70.03Cr, and the preparation steps are as follows:
1. accurately weighing raw material K2CO3 0.5mmol，In2O3 0.485mmol，NH4H2PO4 2mmol，Cr2O30.015mmol；
2. Fully mixing the weighed raw materials, burning the raw materials in air at 1100 ℃ for 10 hours, and cooling the raw materials to room temperature along with a furnace to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at the temperature of 80 ℃ to obtain KIn0.97P2O70.03Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are shown in figure 3, and it can be seen from the figure that the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-800 nm and emits broadband near infrared light in the range of 750-1050 nm.
Example 4:
a phosphate-based phosphor material, the chemical expression of the phosphor is LiSc0.94P2O70.06Cr, and the preparation steps are as follows:
1. accurately weighing raw material Li2CO3 0.575mmol，Sc2O3 0.47mmol，NH4H2PO4 2.1mmol，Cr2O30.03mmol；
2. Fully mixing the weighed raw materials, burning for 2 hours at 1025 ℃ in air, cooling to room temperature along with a furnace, grinding into powder, and repeatedly burning for 2 times to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at the temperature of 80 ℃ to obtain the LiSc0.94P2O70.06Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are shown in figure 4, and it can be seen from the figure that the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-780 nm and emits broadband near-infrared light in the range of 750-1100 nm.
Example 5:
a phosphate-based phosphor material, the chemical expression of the phosphor is LiSc0.9P2O70.1Cr, and the preparation method comprises the following steps:
1. accurately weighing raw material Li2CO3 0.575mmol，Sc2O3 0.45mmol，NH4H2PO4 2.1mmol，Cr2O30.05mmol；
2. Fully mixing the weighed raw materials, burning for 2 hours at 1025 ℃ in air, cooling to room temperature along with a furnace, grinding into powder, and repeatedly burning for 2 times to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at the temperature of 80 ℃ to obtain the LiSc0.9P2O70.1Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are similar to those of embodiment 4, and the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-780 nm and emits broadband near infrared light in the range of 750-1100 nm.
Example 6:
a phosphate-based phosphor material, the chemical expression of the phosphor is LiSc0.937P2O70.06Cr,0.003Yb, prepared by the following steps:
1. accurately weighing raw material Li2CO3 0.575mmol，Sc2O3 0.4685mmol，NH4H2PO4 2.1mmol，Cr2O30.03mmol,Yb2O3 0.0015mmol；
2. Fully mixing the weighed raw materials, burning for 2 hours at 1025 ℃ in air, cooling to room temperature along with a furnace, grinding into powder, and repeatedly burning for 2 times to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at the temperature of 80 ℃ to obtain the LiSc0.937 P2O70.06Cr,0.003Yb phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are shown in fig. 5, and it can be seen from the figure that the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-800 nm and emits broadband near infrared light in the range of 750-1100 nm.
Example 7:
a phosphate-based phosphor material, the chemical expression of the phosphor is LiSc0.89 P2O70.06Cr,0.05Yb, which is prepared by the following steps:
1. accurately weighing raw material Li2CO3 0.575mmol，Sc2O3 0.445mmol，NH4H2PO4 2.1mmol，Cr2O30.03mmol,Yb2O3 0.025mmol；
2. Fully mixing the weighed raw materials, burning for 2 hours at 1025 ℃ in air, cooling to room temperature along with a furnace, grinding into powder, and repeatedly burning for 2 times to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at the temperature of 80 ℃ to obtain the LiSc0.89P2O70.06Cr,0.05Yb phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are shown in fig. 6, and it can be seen from the figure that the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-800 nm, and emits broadband near-infrared light in the range of 900-1000 nm.
Example 8:
a phosphate-based phosphor material, the chemical expression of the phosphor is Li0.95Na0.05Al0.87Ga0.1P2O70.03Cr, and the preparation steps are as follows:
1. accurately weighing raw material Li2CO3 0.475mmol，Na2CO3 0.025mmol,Al2O3 0.435mmol，Ga2O30.05mmol,NH4H2PO4 2mmol，Cr2O3 0.015mmol；
2. Fully mixing the weighed raw materials, burning for 6 hours at 800 ℃ in air, and cooling to room temperature along with a furnace to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at 60 ℃ to obtain the Li0.95Na0.05Al0.87Ga0.1P2O70.03Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are similar to those of embodiment 1, and the fluorescent powder material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-780 nm and emits broadband near infrared light in the range of 750-1000 nm.
Example 9:
a phosphate-based phosphor material, the chemical expression of the phosphor is Li0.95K0.05Sc0.87In0.1P2O70.03Cr, and the preparation steps are as follows:
1. accurately weighing raw material Li2CO3 0.475mmol，K2CO3 0.025mmol,Sc2O3 0.435mmol，In2O30.05mmol,NH4H2PO4 2mmol，Cr2O3 0.015mmol；
2. Fully mixing the weighed raw materials, burning for 2 hours at 1025 ℃ in air, cooling to room temperature along with a furnace, grinding into powder, and repeatedly burning for 2 times to obtain a burning product;
3. fully grinding the obtained roasted product into powder, sieving the powder by a 200-mesh sieve, washing the powder for 3 times by deionized water, and drying the powder at the temperature of 80 ℃ to obtain the Li0.95K0.05Sc0.87In0.1P2O70.03Cr phosphate-based phosphor material.
The excitation spectrum and the emission spectrum of the embodiment are similar to those of embodiment 4, and the phosphor material of the embodiment can be excited by visible light in the ranges of 400-520 nm and 550-780 nm and emits broadband near infrared light in the range of 750-1100 nm.
Where the unexplained elements are referred to as being prior art or being implemented using prior art.
Claims (8)
1. A phosphate-based phosphor material, characterized by: the chemical expression of the fluorescent powder material is AB1-xP2O7xCr, wherein A is at least one of Li, Na and K, and x is more than or equal to 0.01 and less than or equal to 0.1.
2. A phosphate-based phosphor material according to claim 1, wherein: the chemical expression of the fluorescent powder material can also be AB1-x-yP2O7xCr, yYb, wherein A is at least one of Li, Na and K, B is at least one of Al, Ga, In and Sc, x is more than or equal to 0.01 and less than or equal to 0.1, and y is more than 0 and less than or equal to 0.05.
3. A phosphate-based phosphor material according to claim 1 or 2, characterized in that: the fluorescent powder material is excited by visible light in the range of 400-520 nm and 550-780 nm and emits broadband near infrared light in the range of 750-1100 nm.
4. A method of preparing a phosphate-based phosphor material according to claim 1 or 2, characterized in that: the method comprises the following steps:
1) accurately weighing carbonates of Li, Na and K according to the chemical dose ratio of the phosphate-based fluorescent powder materialOxides of Al, Ga, In, Sc and NH4H2PO4As a raw material;
2) fully and uniformly mixing the raw materials weighed in the step 1) to obtain a mixture, and firing the mixture at a high temperature in an air atmosphere to obtain a firing product;
3) grinding the burning product obtained in the step 2) into powder, and then washing and drying to obtain the phosphate-based fluorescent powder material.
5. The method of claim 4, wherein the phosphate-based phosphor material is prepared by: the excess percentage of the Li carbonate in the step 1) is 0-15%, and NH4H2PO4The excess percentage is 0-10%.
6. The method of claim 4, wherein the phosphate-based phosphor material is prepared by: the high-temperature burning condition in the step 2) is as follows: the temperature is 800-1100 ℃, the burning time is 2-10 h, and the burning times are at least 1 time.
7. The method of claim 4, wherein the phosphate-based phosphor material is prepared by: grinding the burning product into powder in the step 3), and then washing and drying, namely grinding the burning product into powder, sieving the powder with a 200-mesh sieve, washing for 1-3 times, centrifuging and drying the precipitate at the temperature of 60-80 ℃.
8. Use of a phosphate-based phosphor material according to claim 1 or 2, characterized in that: the phosphate-based fluorescent powder material can be used for constructing a broadband near-infrared fluorescence conversion type LED device.
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| CN114672310A (en) * | 2020-12-24 | 2022-06-28 | 中国科学院宁波材料技术与工程研究所 | Pyrophosphate near-infrared fluorescent powder and preparation method and application thereof |
| CN113755169B (en) * | 2021-09-30 | 2022-11-01 | 中国科学院长春应用化学研究所 | Phosphate near-infrared luminescent temperature measurement material and preparation method thereof |
| CN116200194B (en) * | 2021-11-30 | 2024-05-14 | 厦门稀土材料研究所 | Near infrared luminescent material, preparation method thereof and LED light source containing luminescent material |
| CN114907852B (en) * | 2022-05-06 | 2024-03-15 | 东南大学 | ScF 3 :Cr 3+ Preparation method and application of near infrared fluorescent powder with less solvent |
| CN114940904B (en) * | 2022-05-23 | 2023-01-31 | 山东大学 | Yb-based short-wave infrared luminescent material and preparation method and application thereof |
| CN115558497A (en) * | 2022-09-20 | 2023-01-03 | 中山大学 | Dy-based composite material 3+ And Tm 3+ Coactivated phosphate material, preparation method and application thereof |
| CN115595152B (en) * | 2022-10-20 | 2023-09-12 | 杭州电子科技大学 | Ga with near infrared emission enhancement 2 O 3 ：Cr 3+ Luminescent material and preparation method thereof |
| CN117070215A (en) * | 2023-08-17 | 2023-11-17 | 广东工业大学 | Phosphate near-infrared luminescent material and preparation method and application thereof |
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| CN108865140A (en) * | 2018-07-16 | 2018-11-23 | 东南大学 | A kind of broad band emitting phosphor material and preparation method thereof |
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