CN111363546A - Near-infrared fluorescent powder with high thermal stability and preparation method and application thereof - Google Patents
Near-infrared fluorescent powder with high thermal stability and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a high-thermal stability near-infrared fluorescent powder, a preparation method and application thereof, wherein the chemical formula of the fluorescent powder is NaRE1‑xMg1‑xWO62xR, wherein the matrix is NaREMgWO6RE is rare earth element Gd or La, and the luminescence center ion R is Cr3+Or Mn2+X is the mole fraction of the luminescence center ion R, 0<x is less than or equal to 0.1 and has two luminescence centers; the material is prepared by a solid-phase sintering method. The emission wavelength of the near-infrared fluorescent powder is 700 nm-1100nm, the emission peak is 800 nm-900 nm, and the light intensity attenuation is less than 15% at 150 ℃. Can be well applied to biological detection, biological imaging and food detection. The solid-phase sintering method adopted by the invention has the advantages of simple preparation process, easy operation and control, high safety, short preparation time and convenience for large-scale production, popularization and application.
Description
Technical Field
The invention relates to a fluorescent powder, in particular to a high-thermal-stability near-infrared fluorescent powder, a preparation method and application thereof, and belongs to the technical field of near-infrared luminescent materials.
Background
Near-infrared (NIR) technology is a new optical technology field, and is receiving attention from researchers due to its special advantages, such as large penetration depth and less interference. With the development of near-infrared technology, near-infrared is extended to many medical fields; pharmacology, molecular cell biology, diagnostics, and the like. For example, the position of blood vessels is detected by near infrared rays harmless to the human body, and distribution images of the blood vessels are projected on the arm in real time so as to let the medical staff know where the needle should be put, which may be free from suffering from "making no dead needle". In addition, the near-infrared fluorescence mark emits light in a near-infrared region, biomolecules do not emit light in the near-infrared region and have no spectrum overlapping interference, the near-infrared fluorescence mark can be excited by visible light with shorter wavelength, so that the excitation light is prevented from being scattered, higher sensitivity is obtained, the penetration depth of near-infrared light in living biological tissues is large, light signals can be generated in deep tissues, almost no influence is caused on the tissues, and the development of the technologies such as medical imaging, tumor treatment and the like is facilitated. Besides, the near infrared light can be applied to measuring the moisture, fat, carbohydrate, sugar or protein content in food in the food industry, agriculture and other industries. However, the technology relies on near-infrared fluorescent powder capable of emitting wide spectrum, and most of the existing near-infrared fluorescent powder cannot meet the use requirements, so that more near-infrared fluorescent powder with wide-band excitation and wide-emission spectrum needs to be researched and developed, and more choices are provided for using the near-infrared fluorescent powder in food detection, biological detection and organism imaging.
Near infrared pc-LEDs will overcome the inherent limitations of conventional incandescent or tungsten halogen lamps (inefficient, large size) and near infrared led (narrow FWHM), while exhibiting relatively high energy efficiency, wide FWHM, compact size and excellent durability. The unique advantages of near infrared pc-LEDs make them well suited for spectroscopic applications. In particular NIR pc-LEDs with 780-1100nm radiation. When designing the broadband near-infrared fluorescent powder, the reasonable selection of the luminous center is the key. Eu having 4f-5d transition2+And Ce3+Ions generally have a broad emission in the ultraviolet or visible region of the spectrum. Trivalent lanthanum ion (Pr)3+、Nd3+、Sm3+) The doped material is capable of producing near infrared radiation, but has a narrow spectral bandwidth and low excitation efficiency (non-patent reference appl. phy. express7(2014)072601.j.lumin.172(2016)185-190.j.mater.chem.c 7(2019) 4320-. And the transition metal Cr in the weak octahedral crystal field3+The ions exhibit broadband long wavelength radiation. Thus, Cr3+Activating phosphors recently attracted more and more interest for applications dominated by near-infrared pc.
Patent application CN108531175A provides a near-infrared phosphor, which has a chemical formula: mg (magnesium)3- xGa2CrxGeO8，0<x is less than or equal to 0.1, the emission peak of the fluorescent powder is weaker in 850nm-1100nm, and the raw material containing Ga is easy to decompose at high temperature, so that the industrial application of the fluorescent powder is greatly limited. Patent application CN108865140A discloses a broadband emitting phosphor material, the chemical formula of which is Ca3Sc2-xSi3O12:xCr，0<x is less than or equal to 0.1. Although the emission band of the fluorescent powder is wide, the absorption of the excitation wavelength at 500-600nm is extremely weak, and the emission waveThe narrow-band emission at 900-. Patent application CN106433643A discloses titanate near-infrared fluorescent powder and preparation method thereof, and the chemical formula of the fluorescent powder is A(2-x)MgTi(l-y)O6xYb, yMn, wherein A is Gd3+、La3+Or Y3+X is more than or equal to 0.03 and less than or equal to 0.18, and y is more than or equal to 0.001 and less than or equal to 0.004. The phosphor emission band is in the range of 900-.
Disclosure of Invention
The invention aims to provide a high-thermal stability near-infrared fluorescent powder which has a wider emission band.
The invention also aims to provide the preparation method of the near-infrared fluorescent powder with high thermal stability, which has simple preparation process and is easy for (semi-) industrial production.
The invention also aims to provide the application of the high-thermal stability near-infrared fluorescent powder.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a high-thermal stability near-infrared fluorescent powder with a chemical formula of NaRE1-xMg1-xWO62xR, wherein the matrix is NaREMgWO6RE is rare earth element Gd or La, and the luminescence center ion R is Cr3+Or Mn2+X is the mole fraction of the luminescence center ion R, 0<x is less than or equal to 0.1; the near-infrared fluorescent powder has two luminous centers.
The emission wavelength of the near-infrared fluorescent powder is in the range of 700 nm-1100nm, the main emission peak is 800 nm-900 nm, and the near-infrared fluorescent powder can be excited by a blue light chip with the wavelength of 430 nm-460 nm.
The luminous intensity of the near-infrared fluorescent powder is reduced along with the increase of the temperature, but the luminous intensity of the near-infrared fluorescent powder is attenuated by less than 15% at the ambient temperature of 150 ℃.
The invention also provides a preparation method of the high-thermal stability near-infrared fluorescent powder, which adopts a solid-phase sintering method and specifically comprises the following steps:
(1) according to the chemical formula NaRE1-xMg1-xWO6:2xR，0<x≤01, weighing raw material powder containing Na element, RE element, Mg element, W element and R element according to the stoichiometric ratio of each element, mixing the raw material powder, a dispersing agent, a ball-milling medium, a charge compensation agent and alumina grinding balls according to a certain proportion, and putting the mixture into a ball-milling tank for ball-milling to obtain mixed slurry;
(2) placing the mixed slurry subjected to ball milling in the step (1) into a drying oven for drying, sieving the dried mixed powder, and placing the sieved mixed powder into a tubular furnace for calcining under argon atmosphere to remove organic matters;
(3) and (3) sintering the powder prepared in the step (2) in a tube furnace under the argon atmosphere at the sintering temperature of 1200-1500 ℃ for 2-4 h, taking out the sintered powder, fully grinding and sieving to obtain the high-thermal-stability near-infrared fluorescent powder.
Preferably, in the step (1), the raw material powder is an oxide or carbonate containing corresponding elements, the mass percentage purity is more than or equal to 99.99%, and the average particle size is 10nm to 50 nm.
Preferably, in step (1), the charge compensator is LiF or CaF2The addition amount of the charge compensation agent is 0.5-1 time of the molar weight of the luminescence center ions, the mass percentage purity of the charge compensation agent is 99.9-99.999%, and the average particle size is 1-100 nm.
Preferably, in the step (1), the dispersant is polyetherimide, and the dosage of the dispersant is 0.5-1.5% of the total mass of the raw materials.
Preferably, in the step (1), the ball milling rotation speed is 200r/min to 250r/min, and the ball milling time is 10h to 15 h.
Preferably, in the step (2), the sintering temperature is 500-600 ℃, the heat preservation time is 5-10 h, the temperature rise rate during sintering is 2-4 ℃/min, and the temperature reduction rate after sintering is 2-4 ℃/min.
Preferably, in the step (3), the temperature rising rate during sintering is 1-2 ℃/min, and the temperature lowering rate after sintering is 1-2 ℃/min.
Preferably, in the step (2) and the step (3), the number of the sieved meshes is 50-100 meshes, and the sieving frequency is 3-5 times.
The invention also provides application of the high-thermal stability near-infrared fluorescent powder in biological detection, organism imaging and food detection.
The emission wavelength of the near-infrared fluorescent powder is 700 nm-1100nm, the emission main peak is 800 nm-900 nm, the near-infrared fluorescent powder can be effectively excited by a blue light (430 nm-460 nm) chip, and the near-infrared fluorescent powder and the blue light chip are packaged into a remote excitation mode, so that the near-infrared fluorescent powder can be applied to biological detection, organism imaging and food detection.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts transition Cr or Mn element, and adds in matrix NaREMgWO6The obtained near-infrared fluorescent powder has two luminous centers, and the emission spectrum width can be effectively adjusted.
(2) The near-infrared fluorescent powder provided by the invention has the emission wavelength of 700-1100 nm and the main emission peak of 800-900 nm, can be effectively excited by a blue light (430-460 nm) chip, is packaged with the blue light chip into a remote excitation mode, and can be applied to biological detection, organism imaging and food detection.
(3) The near-infrared fluorescent powder provided by the invention has the advantages that the luminous intensity attenuation is less than 15% at the ambient temperature of 150 ℃, and the thermal stability is high.
Drawings
FIG. 1 is an XRD pattern of a near-infrared phosphor prepared in examples 1 to 3 of the present invention;
FIG. 2 is an excitation spectrum of a near-infrared phosphor prepared in example 1 of the present invention under the monitoring of a wavelength of 880 nm;
FIG. 3 is an emission spectrum of a near-infrared phosphor prepared in example 1 of the present invention under a laser having a wavelength of 460 nm;
FIG. 4 is an emission spectrum of a near-infrared phosphor prepared in example 1 according to the present invention with temperature.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
The raw material powder used in the following examples is a commercial product, the mass percentage purity is more than 99.99%, and the average particle size is 10 nm-50 nm; the mass percentage purity of the used charge compensation agent is 99.9-99.999%, and the average grain diameter is 1-100 nm.
Example 1: the chemical formula of the preparation is NaGd0.995Mg0.995WO6:0.01Cr3+Near-infrared fluorescent powder
(1) Setting the mass of a target product to be 60g, and respectively weighing sodium oxide, gadolinium oxide, chromium oxide, magnesium oxide and tungsten oxide as raw material powder according to the stoichiometric ratio of each element in the chemical formula; adding raw material powder, 0.03g of PEI, 0.0128g of charge compensation agent LiF and 120g of absolute ethyl alcohol into a ball milling tank, adding 120g of alumina balls, and carrying out ball milling, wherein the ball milling rotating speed is 200r/min, and the ball milling time is 15 hours;
(2) placing the mixed slurry subjected to ball milling in the step (1) into a forced air drying oven for drying, sieving the dried mixed powder with a 50-mesh sieve for 3 times, calcining under argon atmosphere to remove residual organic matters, wherein the calcining temperature is 500 ℃, the calcining time is 5 hours, the heating rate is 2 ℃/min, and the cooling rate after sintering is 2 ℃/min;
(3) placing the powder prepared in the step (2) into an argon tube type furnace for atmosphere sintering, wherein the sintering temperature is 1200 ℃, the heat preservation time is 2h, the heating rate is 1 ℃/min, and the cooling rate after sintering is 1 ℃/min; and (3) fully grinding the sintered near-infrared fluorescent powder in an agate mortar, sieving by a 50-mesh sieve, and sieving for 3 times to obtain the near-infrared fluorescent powder.
The NaGd obtained in the example was used0.995Mg0.995WO6:0.01Cr3+XRD test is carried out on the near-infrared fluorescent powder, and the test result is shown in figure 1, which shows that: the prepared material is double perovskite pure phase, and luminescent ion Cr3+Into the crystal lattice of the matrix, the crystal structure and NaGdMgWO6The same is true.
The NaGd obtained in the example was used0.995Mg0.995WO6:0.01Cr3+The excitation spectrum test of the near-infrared fluorescent powder is carried out under the monitoring of the wavelength of 880nm, the result is shown in figure 2, which shows that the near-infrared fluorescent powder has two absorption bands respectively positioned near 460nm and 670nm, which indicates that the near-infrared fluorescent powder has two emissionsA center.
The NaGd obtained in the example was used0.995Mg0.995WO6:0.01Cr3+The near infrared fluorescent powder is subjected to an excitation emission spectrum test at the wavelength of 460nm, and as shown in FIG. 3, the result shows that the main emission peak is near 880 nm.
FIG. 4 shows NaGd obtained in this example0.995Mg0.995WO6:0.01Cr3+And the emission spectrogram of the near-infrared fluorescent powder along with the temperature change. The results show that: the luminous intensity of the fluorescent powder is gradually reduced along with the increase of the temperature, but the luminous intensity is not obviously reduced along with the increase of the temperature within the range of room temperature to 150 ℃, and the luminous intensity is attenuated by 9.8% at 150 ℃.
Example 2: preparation of a chemical formula of NaLa0.99Mg0.99WO6:0.02Cr3+Near-infrared fluorescent powder
(1) Setting the mass of a target product to be 60g, and respectively weighing sodium oxide, lanthanum oxide, chromium oxide, magnesium oxide and tungsten oxide as raw material powder according to the stoichiometric ratio of each element in the chemical formula; mixing the raw material powder, 0.09g of PEI, 0.101g of charge compensation agent CaF2Adding 180g of absolute ethyl alcohol into a ball milling tank, adding 120g of alumina balls, and carrying out ball milling, wherein the ball milling rotation speed is 250r/min, and the ball milling time is 10 h;
(2) placing the mixed slurry subjected to ball milling in the step (1) into a forced air drying oven for drying, sieving the dried mixed powder with a 100-mesh sieve for 5 times, calcining under argon atmosphere to remove residual organic matters, wherein the calcining temperature is 600 ℃, the calcining time is 10 hours, the heating rate is 4 ℃/min, and the cooling rate after sintering is 4 ℃/min;
(3) placing the powder prepared in the step (2) into an argon tube type furnace for atmosphere sintering, wherein the sintering temperature is 1500 ℃, the heat preservation time is 4h, the heating rate is 2 ℃/min, and the cooling rate after sintering is 2 ℃/min; and (3) fully grinding the sintered near-infrared fluorescent powder in an agate mortar, sieving by a 100-mesh sieve, and sieving for 5 times to obtain the near-infrared fluorescent powder.
The NaLa obtained in this example was used0.99Mg0.99WO6:0.02Cr3+Near infrared phosphor powderThe XRD test is carried out, and the test result is shown in figure 1, which shows that: the prepared material is double perovskite pure phase, and luminescent ion Cr3+Into the crystal lattice of the matrix, the crystal structure and NaLaMgWO6The same is true.
The NaLa obtained in this example was used0.99Mg0.99WO6:0.02Cr3+The near-infrared fluorescent powder is subjected to excitation emission spectrum test at the wavelength of 460nm, and the result shows that the main emission peak is located near 891 nm.
The NaLa obtained in this example was used0.99Mg0.99WO6:0.02Cr3+And (3) carrying out emission spectrum test on the near-infrared fluorescent powder along with temperature change. The results show that: the luminous intensity of the phosphor gradually decreased with increasing temperature, but the luminous intensity was attenuated by 13.4% at 150 ℃.
Example 3: the chemical formula of the preparation is NaGd0.995Mg0.995WO6:0.01Mn2+Near-infrared fluorescent powder.
(1) Setting the mass of a target product to be 60g, and respectively weighing sodium oxide, gadolinium oxide, chromium oxide, magnesium oxide, tungsten oxide and manganese carbonate as raw material powder according to the stoichiometric ratio of each element in the chemical formula; adding raw material powder, 0.06g of PEI, 0.0322g of charge compensation agent LiF and 150g of absolute ethyl alcohol into a ball milling tank, adding 120g of alumina balls, and carrying out ball milling, wherein the ball milling rotating speed is 220r/min, and the ball milling time is 15 h;
(2) placing the mixed slurry subjected to ball milling in the step (1) into a forced air drying oven for drying, sieving the dried mixed powder with an 80-mesh sieve for 4 times, calcining under argon atmosphere to remove residual organic matters, wherein the calcining temperature is 540 ℃, the calcining time is 10 hours, the heating rate is 3 ℃/min, and the cooling rate after sintering is 3 ℃/min;
(3) placing the powder prepared in the step (2) into an argon tube type furnace for atmosphere sintering, wherein the sintering temperature is 1400 ℃, the heat preservation time is 3h, the heating rate is 2 ℃/min, and the cooling rate after sintering is 2 ℃/min; and (3) fully grinding the sintered near-infrared fluorescent powder in an agate mortar, sieving by a 80-mesh sieve, and sieving for 4 times to obtain the near-infrared fluorescent powder.
Will make the present implementationNaGd obtained in examples0.995Mg0.995WO6:0.01Mn2+XRD test is carried out on the near-infrared fluorescent powder, and the test result is shown in figure 1, which shows that: the prepared material is double perovskite pure phase, and luminescent ions Mn2+Into the crystal lattice of the matrix, the crystal structure and NaGdMgWO6The same is true.
The NaGd obtained in the example was used0.995Mg0.995WO6:0.01Mn2+The near-infrared fluorescent powder is subjected to excitation emission spectrum test at the wavelength of 460nm, and the result shows that the main emission peak is positioned near 870 nm.
NaGd obtained in the example was used0.995Mg0.995WO6:0.01Mn2+And (3) carrying out emission spectrum test on the near-infrared fluorescent powder along with temperature change. The results show that: the emission intensity of the phosphor gradually decreased as the temperature increased, but the emission intensity was attenuated by 13% at 150 ℃.
Claims (10)
1. The high-thermal stability near-infrared fluorescent powder is characterized in that the chemical formula of the fluorescent powder is NaRE1-xMg1-xWO62xR, wherein the matrix is NaREMgWO6RE is rare earth element Gd or La, and the luminescence center ion R is Cr3+Or Mn2+X is the mole fraction of the luminescence center ion R, 0<x is less than or equal to 0.1; the near-infrared fluorescent powder has two luminescence centers, the emission wavelength is in the range of 700 nm-1100nm, the main emission peak is 800 nm-900 nm, and the near-infrared fluorescent powder can be excited by a blue light chip with the wavelength of 430 nm-460 nm.
2. A highly thermally stable near-infrared phosphor as claimed in claim 1, wherein the luminous intensity of said near-infrared phosphor decays less than 15% at an ambient temperature of 150 ℃.
3. A method for preparing the near-infrared fluorescent powder with high thermal stability as claimed in claim 1 or 2, wherein the sintering is carried out by a solid-phase reaction method, which comprises the following steps:
(1) according to the chemical formula NaRE1-xMg1-xWO6:2xR，0<The stoichiometric ratio of each element in x is less than or equal to 0.1, weighing raw material powder containing Na element, RE element, Mg element, W element and R element respectively, mixing the raw material powder, dispersing agent, ball milling medium, charge compensation agent and alumina grinding balls according to a certain proportion, and putting the mixture into a ball milling tank for ball milling to obtain mixed slurry;
(2) placing the mixed slurry subjected to ball milling in the step (1) into a drying oven for drying, sieving the dried mixed powder, and placing the sieved mixed powder into a tubular furnace for calcining under argon atmosphere to remove organic matters;
(3) and (3) sintering the powder prepared in the step (2) in a tube furnace under the argon atmosphere at the sintering temperature of 1200-1500 ℃ for 2-4 h, taking out the sintered powder, fully grinding and sieving to obtain the high-thermal-stability near-infrared fluorescent powder.
4. The method for preparing near-infrared fluorescent powder with high thermal stability according to claim 3, wherein in the step (1), the raw material powder is oxide or carbonate containing corresponding elements, the mass percentage purity is not less than 99.99%, and the average particle size is 10nm to 50 nm.
5. A method for preparing high thermal stability near infrared phosphor as claimed in claim 3, wherein in step (1), said charge compensator is LiF or CaF2The addition amount of the charge compensation agent is 0.5-1 time of the molar weight of the luminescence center ions, the mass percentage purity of the charge compensation agent is 99.9-99.999%, and the average particle size is 1-100 nm.
6. The method for preparing near-infrared phosphor with high thermal stability according to claim 3, wherein in step (1), the dispersant is polyetherimide, and the amount of the dispersant is 0.5-1.5% of the total mass of the raw material powder.
7. The method for preparing a near-infrared phosphor with high thermal stability according to claim 3, wherein in the step (1), the ball milling rotation speed is 200r/min to 250r/min, and the ball milling time is 10h to 15 h.
8. The method for preparing a near-infrared phosphor with high thermal stability as claimed in claim 3, wherein in the step (2), the sintering temperature is 500 ℃ to 600 ℃, the holding time is 5h to 10h, the temperature rising rate during sintering is 2 ℃/min to 4 ℃/min, and the temperature falling rate after sintering is 2 ℃/min to 4 ℃/min.
9. The method for preparing a near-infrared phosphor with high thermal stability as claimed in claim 3, wherein in the step (2) and the step (3), the mesh number of the sieved mesh is 50-100 meshes, and the sieving frequency is 3-5 times.
10. Use of the high thermal stability near infrared phosphor of claim 1 or 2 for biological detection, biological imaging and food detection.
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| CN115520894B (en) * | 2022-10-26 | 2024-02-13 | 中国科学院长春应用化学研究所 | Near infrared luminescent material, preparation method thereof and luminescent device |
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