CN109913214B - Far-infrared and near-infrared emission fluoride fluorescent material and preparation and application thereof - Google Patents

Far-infrared and near-infrared emission fluoride fluorescent material and preparation and application thereof Download PDF

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CN109913214B
CN109913214B CN201910226475.5A CN201910226475A CN109913214B CN 109913214 B CN109913214 B CN 109913214B CN 201910226475 A CN201910226475 A CN 201910226475A CN 109913214 B CN109913214 B CN 109913214B
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CN109913214A (en
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邵起越
彭瑾
丁浩
董岩
蒋建清
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Southeast University
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Abstract

The invention discloses a far-infrared and near-infrared emission fluoride fluorescent material, and preparation and application thereof, wherein the chemical expression of the fluorescent powder material is RxAl1‑yFx+3yCr; wherein R is at least one of Li, Na, K, Rb or Cs, x is more than or equal to 1 and less than or equal to 3, and y is more than or equal to 0.005 and less than or equal to 0.2. The preparation method comprises the following steps: 1) weighing AlF according to the chemical composition and stoichiometric ratio of the fluorescent material3、CrF3R-containing fluoride and NH4F; 2) fully grinding and uniformly mixing the weighed raw materials, and then firing at a high temperature to obtain a roasted product; 3) and grinding the roasted product into powder, washing, centrifuging and drying to obtain the fluorescent material. The fluorescent material has stable chemical property and excellent luminous performance, can be excited by a blue light or red light LED chip, has simple preparation operation, no pollution and low cost, and can be used for packaging and manufacturing far-red and near-infrared emission fluorescence conversion type LED devices.

Description

Far-infrared and near-infrared emission fluoride fluorescent material and preparation and application thereof
Technical Field
The invention relates to a far-infrared and near-infrared emission fluoride fluorescent material, and preparation and application thereof, and belongs to the technical field of solid luminescent materials.
Background
Photosynthesis is one of the essential conditions for plant growth and development. Researches show that the absorption spectrums of green plants on visible light are basically the same, the absorption spectrums are mainly concentrated in a 400-500 nm purple blue area and a 600-800 nm red light area, blue light can promote stem and leaf growth, and red light can regulate flowering periods, so that the blue light and the red light have important effects on plant growth, development, flowering and fruiting. Economic crops such as vegetables, flowers and the like in the greenhouse are obviously affected by seasons and severe weather, and the lack of illumination plays an important role in slowing down the growth of the economic crops, so that certain illumination is required to supplement the economic crops. Although the single infrared light (800-. At the present stage, traditional light sources such as fluorescent lamps, metal halide lamps, high-pressure sodium lamps and incandescent lamps are mainly adopted as plant growth lamps in indoor planting, the spectrums of the light sources are continuous composite light, the proportion of various light cannot be adjusted, and the light sources generally lack far-red light and near-infrared light of 700-950 nm, so that the light sources are not matched with light required by plant growth, and the efficiency of promoting the plant growth is low.
With the rapid development of white light LED technology and the scale effect and cost advantage which are mature day by day, the LED plant growth lamp obtained by exciting fluorescent powder by adopting a blue light chip has rich and adjustable spectrum and can be matched with light required by plant growth; meanwhile, the blue light chip has the advantages of small heat, small volume, high power, low cost and the like, and the fluorescence conversion type LED plant growth lamp can meet the requirements of low heat load, production space miniaturization and the like, and has wide application prospect. At present, the luminous materials emitting at 700 nm-950 nm in the market are relatively few, so that the far-infrared and near-infrared emission fluorescent powder with wide waveband, no toxicity and moderate price is developed and the proper plant growth lamp is prepared, which has very important significance for the development of high-efficiency green agriculture in China.
Disclosure of Invention
The technical problem is as follows: aiming at the defects of the prior art, the invention provides a far-red and near-infrared emission fluoride fluorescent material, and preparation and application thereof, wherein the material has stable chemical property and excellent luminous performance, can be effectively excited by blue light (380 nm-480 nm) or red light (550-700 nm), and emits far-red and near-infrared light in the range of 700 nm-900 nm; the preparation method is simple, easy to operate, pollution-free and low in cost, and can be combined with different LED chips to construct the far-red and near-infrared emission fluorescence conversion type LED plant growth lamp to promote plant growth.
The technical scheme is as follows: the invention provides a far-infraredAnd near-infrared emission fluoride fluorescent material, wherein the chemical expression of the fluorescent material is RxAl1-yFx+3yCr, wherein R is at least one of Li, Na, K, Rb or Cs, x is more than or equal to 1 and less than or equal to 3, and y is more than or equal to 0.005 and less than or equal to 0.2.
Wherein:
the fluorescent material is effectively excited by blue light with the wavelength range of 380 nm-480 nm or red light with the wavelength range of 550-700 nm, and emits far-red light and near-infrared light with the wavelength range of 700 nm-900 nm.
The invention also provides a preparation method of the far-infrared and near-infrared emission fluoride fluorescent material, which comprises the following steps:
1) weighing the following raw materials according to the chemical composition and the stoichiometric ratio of the fluorescent material: AlF3、CrF3And R-containing fluorides;
2) fully grinding and uniformly mixing the raw materials weighed in the step 1), and then firing at a high temperature to obtain a roasted product;
3) grinding the roasted product obtained in the step 2) into powder, washing, centrifuging and drying to obtain the far-red and near-infrared emission fluoride fluorescent material.
Wherein:
the corresponding raw materials in the step 1) also comprise NH4And F, wherein the weighed amount of the F is 0-100% of the total weight of other raw materials.
In the high-temperature burning in the step 2), the burning temperature is 400-900 ℃, the burning time is 1-48 h, and the burning frequency is at least one time.
In the high-temperature burning in the step 2), the atmosphere in the burning process is at least one of vacuum, argon and nitrogen.
Grinding the roasted product into powder in the step 3), wherein the powder is sieved by a 200-400-mesh sieve.
In the drying after the washing centrifugation in the step 3), the used washing agent is ionized water, the washing times are 1-3 times, and the drying temperature is 80-150 ℃.
The invention also provides application of the far-red and near-infrared emission fluoride fluorescent material, the fluorescent material is combined with different LED chips, and the fluorescent material is combined with different LED chips and packaged to prepare far-red and near-infrared emission fluorescence conversion type LED devices.
Wherein:
the far-infrared and near-infrared emission fluorescence conversion type LED device comprises a far-infrared and near-infrared emission fluorescence conversion type LED plant growth lamp.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
1. the far-red and near-infrared emission fluoride fluorescent material provided by the invention has a wide excitation range, can be excited by light in the ranges of 380-480 nm and 550-700 nm, and emits deep red and near-infrared light in the range of 700-900 nm;
2. the preparation method of the far-infrared and near-infrared emission fluoride fluorescent material provided by the invention is simple and easy to operate;
3. the far-red and near-infrared emission fluoride fluorescent material provided by the invention can be combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Drawings
FIG. 1 shows the excitation and emission spectra of far-red and near-infrared emission fluoride fluorescent materials prepared in example 1 of the present invention, with monitoring wavelength and excitation wavelength of 765nm and 450nm, respectively;
FIG. 2 shows the excitation spectra of the far-red and near-infrared emission fluoride fluorescent materials prepared in example 2 of the present invention, with a monitoring wavelength of 740 nm;
FIG. 3 shows the emission spectra of the far-red and near-infrared emission fluoride fluorescent materials prepared in example 2 of the present invention, with the excitation wavelength of 450 nm;
FIG. 4 shows the excitation spectra of the far-red and near-infrared emission fluoride fluorescent materials prepared in example 3 of the present invention, with a monitoring wavelength of 740 nm;
FIG. 5 shows the emission spectra of the far-red and near-infrared emitting fluoride fluorescent materials prepared in example 3 of the present invention, with the excitation wavelength of 450 nm.
Detailed Description
The technical solution of the present invention is further described with reference to the accompanying drawings and the detailed description.
Example 1:
a far-infrared and near-infrared emitting fluoride fluorescent material has a chemical expression of K3Al0.98F60.02Cr, and the preparation steps are as follows:
1. weighing raw material KF.2H2O 0.03mol，AlF3·3H2O 0.0098mol，CrF30.0002mol, weighing NH with the total weight of 20 percent of the raw materials4F；
2. Fully mixing the weighed raw materials, and sintering at 750 ℃ for 3 hours in an argon atmosphere to obtain a roasted 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 K of the invention3Al0.98F60.02Cr fluorescent powder.
The excitation spectrum and emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are shown in fig. 1.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 2:
a far-red and near-infrared emitting fluoride-based fluorescent material has a chemical expression of Na3Al0.96F60.04Cr, and the preparation steps are as follows:
1. weighing raw materials NaF 0.03mol and AlF3·3H2O 0.0096mol，CrF30.0004mol, weighing NH with the total weight of 20 percent of the raw materials4F；
2. Fully mixing the weighed raw materials, and sintering at 700 ℃ for 2 hours in an argon atmosphere to obtain a roasted product;
3. grinding the obtained roasted product into powder, sieving the powder with a 200-mesh sieve, washing the powder for 3 times by using deionized water, and drying the powder at the temperature of 100 ℃ to obtain the Na of the invention3Al0.96F60.04Cr fluorescent powder.
The excitation spectrum and the emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are shown in fig. 2 and 3.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 3:
a far-red and near-infrared emitting fluoride-based fluorescent material has a chemical expression of Na2.5Li0.5Al0.98F60.02Cr, and the preparation steps are as follows:
1. weighing raw materials of 0.025mol of NaF, 0.005mol of LiF and AlF3·3H2O 0.0098mol，CrF30.0002mol, weighing NH accounting for 30 percent of the total weight of the raw materials4F；
2. Fully mixing the weighed raw materials, and sintering for 5 hours at 720 ℃ in an argon atmosphere to obtain a roasted product;
3. grinding the obtained roasted product into powder, sieving the powder with a 200-mesh sieve, washing the powder for 3 times by using deionized water, and drying the powder at the temperature of 100 ℃ to obtain the Na of the invention2.5Li0.5Al0.98F60.02Cr fluorescent powder.
The excitation spectrum and the emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are shown in fig. 3 and 4.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 4:
a far-infrared and near-infrared emitting fluoride-based fluorescent material, the chemical expression of the fluorescent powder is Li3Al0.95F60.05Cr, and the preparation steps are as follows:
1. weighing raw materials LiF 0.03mol and AlF3·3H2O 0.0095mol，CrF3 0.0005mol；
2. Fully mixing the weighed raw materials, and sintering for 5 hours at 720 ℃ in an argon atmosphere to obtain a roasted product;
3. 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 100 ℃ to obtain the Li3Al0.95F60.05Cr fluorescent powder.
The excitation spectrum and the emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 3.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 5:
a far-infrared and near-infrared emitting fluoride-based phosphor material, the chemical expression of the phosphor is KAl0.995F40.005Cr, and the preparation method comprises the following steps:
1. weighing raw material KF.2H2O 0.01mol，AlF3 0.00995mol，CrF30.00005mol, weighing NH with the weight percent of 10 percent of the total weight of the raw materials4F；
2. Fully mixing the weighed raw materials, and sintering at 600 ℃ for 10 hours in vacuum to obtain a roasted product;
3. 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 100 ℃ to obtain the KAl of the invention0.995F40.005Cr fluorescent powder.
The excitation spectrum and emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 1.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 6:
a far-infrared and near-infrared emitting fluoride-based phosphor material, the chemical expression of the phosphor is Na2.5Cs0.5Al0.96F40.04Cr, and the preparation steps are as follows:
1. weighing raw materials of 0.025mol of NaF, 0.005mol of CsF and AlF3 0.0096mol，CrF30.0004mol, weighing NH with the weight percent of the total weight of the raw materials being 80 percent4F；
2. Fully mixing the weighed raw materials, sintering for 2 hours at 400 ℃ in an argon atmosphere, fully grinding a sintered product, and performing secondary firing for 5 hours at 800 ℃ in the argon atmosphere to obtain a roasted product;
3. grinding the roasted 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 the temperature of 150 ℃ to obtain the Na of the invention2.5Cs0.5Al0.96F40.04Cr fluorescent powder.
The excitation spectrum and the emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 2.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 7:
a far-infrared and near-infrared emitting fluoride-based fluorescent powder material has a chemical expression of K2NaAl0.98F60.02Cr, and the preparation steps are as follows:
1. weighing raw material KF.2H2O 0.02mol，NaF 0.01mol，AlF3·3H2O 0.0098mol，CrF30.0002mol；
2. Fully mixing the weighed raw materials, and sintering at 750 ℃ for 2 hours in vacuum to obtain a roasted product;
3. grinding the roasted product into powder, sieving the powder by a 300-mesh sieve, washing the powder for 2 times by deionized water, and drying the powder at the temperature of 100 ℃ to obtain the K of the invention2NaAl0.98F60.02Cr fluorescent powder.
The excitation spectrum and emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 1.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 8:
a far-infrared and near-infrared emitting fluoride-based fluorescent powder material has a chemical expression of K2Al0.94F50.06Cr, and the preparation steps are as follows:
1. weighing raw materials of KF 0.02mol and AlF3 0.0094mol，CrF30.0006mol, weighing NH accounting for 100 percent of the total weight of the raw materials4F；
2. Fully mixing the weighed raw materials, sintering for 2 hours at 500 ℃ in a nitrogen atmosphere, fully grinding a sintered product, and performing secondary firing for 5 hours at 900 ℃ in the nitrogen atmosphere to obtain a roasted product;
3. grinding the roasted product into powder, sieving the powder with a 400-mesh sieve, washing the powder for 3 times by using deionized water, and drying the powder at the temperature of 80 ℃ to obtain the K of the invention2Al0.94F50.06Cr fluorescent powder.
The excitation spectrum and emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 1.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 9:
a far-infrared and near-infrared emitting fluoride-based fluorescent powder material has a chemical expression of K2RbAl0.95F60.05Cr, and the preparation steps are as follows:
1. weighing raw materials of KF 0.02mol, RbF 0.01mol and AlF3·3H2O 0.0095mol，CrF30.0005mol, weighing NH with the weight percent of the total weight of the raw materials being 80 percent4F；
2. Fully mixing the weighed raw materials, and sintering for 48 hours at 400 ℃ in a nitrogen atmosphere to obtain a roasted product;
3. grinding the roasted product into powder, sieving with a 250-mesh sieve, washing with deionized water for 3 times, drying at 150 deg.C,namely, K of the present invention is obtained2RbAl0.95F60.05Cr fluorescent powder.
The excitation spectrum and emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 1.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 10:
a far-infrared and near-infrared emitting fluoride-based fluorescent powder material has a chemical expression of K3Al0.9F60.1Cr, and the preparation method comprises the following steps:
1. weighing raw materials of KF 0.03mol and AlF3·3H2O 0.009mol，CrF30.001mol, weighing NH accounting for 50 percent of the total weight of the raw materials4F；
2. Fully mixing the weighed raw materials, sintering the raw materials at 400 ℃ for 2h in vacuum, fully grinding a sintered product, then performing secondary ignition at 800 ℃ for 4h in vacuum, fully grinding the sintered product, and performing tertiary ignition at 800 ℃ for 4h in vacuum to obtain a roasted product;
3. grinding the roasted product into powder, sieving the powder with a 350-mesh sieve, washing the powder for 3 times by using deionized water, and drying the powder at the temperature of 80 ℃ to obtain the K of the invention3Al0.9F60.1Cr fluorescent powder.
The excitation spectrum and emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 1.
The fluorescent material is combined with different LED chips to construct a far-red and near-infrared emission fluorescence conversion type LED plant growth lamp.
Example 11:
a far-infrared and near-infrared emitting fluoride-based phosphor material, the chemical expression of the phosphor is Na2LiAl0.8F60.2Cr, and the preparation steps are as follows:
1. weighing raw materials of 0.02mol of NaF, 0.01mol of LiF and AlF3 0.008mol，CrF3 0.002mol；
2. Fully mixing the weighed raw materials, and sintering for 2 hours at 720 ℃ in an argon atmosphere to obtain a roasted product;
3. fully grinding the 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 Na of the invention2LiAl0.80F60.2Cr fluorescent powder.
The excitation spectrum and the emission spectrum of the far-red and near-infrared emission fluoride fluorescent material obtained in this example are close to those of example 2.
Where the unexplained elements are referred to as being prior art or being implemented using prior art.

Claims (7)

1. A far-red and near-infrared emission fluoride fluorescent material is characterized in that: the chemical expression of the fluorescent material is RxAl1-yFx+3yCr, wherein R is at least one of Li, Na, K, Rb or Cs, x is more than or equal to 1 and less than or equal to 2, and y is more than or equal to 0.005 and less than or equal to 0.2;
the fluorescent material is effectively excited by blue light with the wavelength range of 380 nm-480 nm or red light with the wavelength range of 550-700 nm, and emits far-red light and near-infrared light with the wavelength range of 700 nm-900 nm.
2. A method of preparing the far-red and near-infrared emitting fluoride fluorescent material of claim 1, characterized in that: the method comprises the following steps:
1) weighing the following raw materials according to the chemical composition and the stoichiometric ratio of the fluorescent material: AlF3、CrF3And R-containing fluorides;
2) fully grinding and uniformly mixing the raw materials weighed in the step 1), and then firing at a high temperature to obtain a roasted product;
3) grinding the roasted product obtained in the step 2) into powder, washing, centrifuging and drying to obtain the far-red and near-infrared emission fluoride fluorescent material;
in which the step of1) The corresponding raw materials also comprise NH4And F, wherein the weighed amount of the F is less than or equal to the total weight of other raw materials.
3. The method of claim 2, wherein the method comprises the steps of: in the high-temperature burning in the step 2), the burning temperature is 400-900 ℃, the burning time is 1-48 h, and the burning frequency is at least one time.
4. The method of claim 2, wherein the method comprises the steps of: in the high-temperature burning in the step 2), the atmosphere in the burning process is at least one of vacuum, argon and nitrogen.
5. The method of claim 2, wherein the method comprises the steps of: grinding the roasted product in the step 3) into powder, wherein the powder is sieved by a 200-400-mesh sieve.
6. The method of claim 2, wherein the method comprises the steps of: in the drying after the washing centrifugation in the step 3), the used detergent is deionized water, the washing times are 1-3 times, and the drying temperature is 80-150 ℃.
7. Use of the far-red and near-infrared emitting fluoride fluorescent material of claim 1, wherein: the fluorescent material is combined with different LED chips and packaged to form a far-red and near-infrared emission fluorescence conversion type LED device;
the far-infrared and near-infrared emission fluorescence conversion type LED device comprises a far-infrared and near-infrared emission fluorescence conversion type LED plant growth lamp.
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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

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