CN110724531A - Spectrum-adjustable red-blue dual-emission europium-doped aluminate fluorescent powder for LED and preparation method thereof - Google Patents
Spectrum-adjustable red-blue dual-emission europium-doped aluminate fluorescent powder for LED and preparation method thereof Download PDFInfo
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- CN110724531A CN110724531A CN201911181303.7A CN201911181303A CN110724531A CN 110724531 A CN110724531 A CN 110724531A CN 201911181303 A CN201911181303 A CN 201911181303A CN 110724531 A CN110724531 A CN 110724531A
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
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Abstract
The invention relates to a spectrum-adjustable red-blue dual-emission europium-doped aluminate fluorescent powder, which has the following chemical expression: CaY2‑xAl4SiO12xEu, wherein x is 0.001-0.05. The invention has the beneficial effects that: the synthesis temperature is low, the required calcination time is short, the preparation steps are simple, and the operation is easy; the prepared fluorescent powder has high purity and high efficiency, is singly doped, saves the cost and does not have the problem of reducing the efficiency of multi-phase and multi-doped fluorescent powder; under the excitation of ultraviolet light of 230-375 nm, blue light of 420 nm as a main peak and red light of 615 nm as a main peak can be emitted; the red-blue double-emission color tunable filter has a wide excitation spectrum, can be well matched with ultraviolet LED chips with different emission wavelengths, and has the characteristics of red-blue double emission and adjustability, so that the red-blue double-emission color tunable filter can be applied to color tuning of display, illumination, plant light supplement and photoluminescence with ultraviolet and near ultraviolet as excitation sources.
Description
Technical Field
The invention belongs to the field of LED luminescent materials, and particularly relates to a red-blue dual-emission europium-doped aluminate fluorescent powder with adjustable spectrum and a preparation method thereof.
Background
As a new generation of solid-state lighting technology, light-emitting diodes (LEDs) have the advantages of long service life, small size, high brightness, high efficiency, environmental friendliness, and the like, and are therefore widely used in the fields of lighting and displaying.
Currently, the most widely used is a combination of a blue LED chip in combination with YAG: Ce yellow phosphor. Because the blue light emitted by the LED chip also participates in the composition of the white light and the deficiency of the red light region of the spectrum causes the defects of high color temperature, low color rendering index and the like, the problem is improved by a method of adding fluorescent powder with partial color lacking in the spectrum, however, the performance of the fluorescent powder excited by the blue light of other colors is poor at present, and the use level is difficult to achieve. On the basis, the scheme that the ultraviolet fluorescent chip is combined with the fluorescent powder is concerned about and widely researched, the ultraviolet fluorescent chip is different from blue light, the fluorescent powder excited by the ultraviolet light is more in types and more abundant in colors, and the problem of blue light harm caused by a high short-wavelength blue light component in the light emission of a blue light LED is solved. However, since the scheme requires the phosphors of three colors of red, green and blue to be mixed into white light, the phosphors emitting in multiple colors need to be provided, the problems of reabsorption, ratio regulation and control, different aging rates caused by the mixing of the multiple phosphors, and efficiency reduction caused by energy transfer among different color light emitting ions of the same phosphor are comprehensively considered, and the phosphors have a new requirement of having more adjustable light emitting colors while adopting less light emitting ion doping.
Under the background, because europium ions with different valence states are rich in emission in a visible spectrum and can be effectively excited by ultraviolet light, the europium ions are often used as single activator ions in ultraviolet excited fluorescent powder, however, the fluorescent powder which has various emission and spectrum-adjustable spectral characteristics is not reported by singly doping europium in an aluminate matrix.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a red-blue dual-emission europium-doped aluminate fluorescent powder with adjustable spectrum and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: spectrum adjustable red blueThe dual-emission europium-doped aluminate fluorescent powder has the following chemical expression: CaY2-xAl4SiO12xEu, wherein x is 0.001-0.05.
A method for preparing spectrum-adjustable red-blue dual-emission europium-doped aluminate fluorescent powder comprises the following steps:
(1) to contain calcium ion Ca2+The compound of (A), yttrium oxide, aluminum oxide, silicon dioxide and europium oxide are used as raw materials, and the chemical expression is CaY2-xAl4SiO12Accurately weighing corresponding raw materials according to the stoichiometric ratio of corresponding elements in xEu, wherein the value range of x is 0.001-0.05, and grinding and uniformly mixing the weighed raw materials to obtain a mixture;
(2) calcining the mixture obtained in the step (1) in an air atmosphere at the temperature of 600-950 ℃ for 1-8 hours;
(3) cooling the calcined mixture to room temperature along with the furnace, grinding and uniformly mixing, and calcining in an air atmosphere at the calcining temperature of 1000-1450 ℃ for 1-8 hours;
(4) and cooling the calcined mixture to room temperature along with the furnace, grinding and uniformly mixing, and calcining in a reducing atmosphere at the calcining temperature of 600-1400 ℃ for 0-8 hours to obtain the red-blue dual-emission aluminate fluorescent powder.
Further, the step (1) contains calcium ions Ca2+The compound (b) is one of calcium oxide and calcium carbonate.
Further, the calcination temperature in the step (2) is preferably 800-900 ℃, and the calcination time is preferably 4-6 hours; the calcination temperature in the step (3) is preferably 1200-1400 ℃, and the calcination time is preferably 4-8 hours; the calcination temperature in the step (4) is preferably 800-1300 ℃, and the calcination time is preferably 1-6 hours.
Further, the reducing atmosphere in the step (4) is one of nitrogen-hydrogen mixed gas, argon-hydrogen mixed gas and carbon monoxide gas.
Further, in the steps (1), (3) and (4), distilled water and/or a volatile organic solvent, which is one of ethanol and acetone, is added during mixing.
The red-blue dual-emission europium-doped aluminate fluorescent powder with adjustable spectrum is applied to illumination, display and photoluminescence chromaticity adjustment with ultraviolet light of 230-375 nanometers as an excitation source, and emits blue light with a main peak of 420 nanometers and red light with a main peak of 615 nanometers.
The invention has the beneficial effects that: (1) the red-blue dual-emission europium-doped aluminate fluorescent powder prepared by the invention can emit blue light with a main peak of 420 nanometers and red light with a main peak of 615 nanometers under the excitation of ultraviolet light with a wavelength of 230-375 nanometers. The red-blue double-emission color tunable filter has a wide excitation spectrum, can be well matched with ultraviolet LED chips with different emission wavelengths, and has the characteristics of red-blue double emission and adjustability, so that the red-blue double-emission color tunable filter can be applied to color tuning of display, illumination, plant light supplement and photoluminescence with ultraviolet and near ultraviolet as excitation sources; (2) the red and blue dual-emission europium-doped aluminate fluorescent powder prepared by the invention can achieve the purpose of adjusting the proportion of red and blue light components in a spectrum only by adjusting the wavelength of an ultraviolet excitation source or the calcining time and temperature in a reducing atmosphere, and can be flexibly adjusted according to the specific requirements during use; (3) the red-blue dual-emission europium-doped aluminate fluorescent powder prepared by the invention is doped with only one activator ion, so that the efficiency reduction caused by energy transfer among various activators is avoided, and the total relative luminous intensity of the fluorescent powder is obviously enhanced along with the increase of the calcining time and temperature in a reducing atmosphere; (4) the red and blue dual-emission europium-doped aluminate fluorescent powder prepared by the invention has the advantages of simple preparation process, low operation difficulty, low requirement on equipment and high purity of the obtained fluorescent powder. The subsequent reduction atmosphere calcination process only needs 1 hour at least, the calcination temperature can be carried out at a low temperature of 800 ℃ at the lowest, the flexibility is high, and the method can be adjusted and adapted according to conditions of actual production equipment and the like.
Drawings
FIG. 1 shows a red-blue dual-emitting europium-doped aluminate phosphor CaY prepared by the present invention1.97Al4SiO120.03Eu X-ray diffraction pattern;
FIG. 2 is a graph of emission spectra of the phosphors prepared in examples 1 and 2 under excitation of 254 nm ultraviolet light;
FIG. 3 is a graph of the emission spectra of the phosphors prepared in examples 2-6 under the excitation of 275 nm ultraviolet light;
FIG. 4 shows the red-blue dual-emitting europium-doped aluminate phosphor CaY prepared by the present invention1.97Al4SiO120.03Eu in the excitation spectrum obtained under the monitoring of light at 420 nm and 615 nm.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings: it should be understood that the preferred embodiments are illustrative of the invention only and are not limiting upon the scope of the invention.
Example 1
According to the formula CaY1.97Al4SiO120.1682g of CaO and Y are respectively weighed according to the stoichiometric ratio of the elements in 0.03Eu2O3:1.3345g、Al2O3:1.2235g、SiO2:0.3605g、Eu2O30.0317 g. The raw materials are put into an agate mortar, absolute ethyl alcohol is used as a dispersion medium to be fully ground and uniformly mixed, then the mixture is placed into a corundum crucible to be calcined for the first time in the air atmosphere, the calcining temperature is 900 ℃, the calcining time is 4 hours, and a sample is taken out after the mixture is naturally cooled to the room temperature. And (3) taking absolute ethyl alcohol as a dispersion medium, grinding and uniformly mixing the mixture after the first calcination, calcining for the second time in an air atmosphere at the calcining temperature of 1400 ℃ for 5 hours, and naturally cooling to room temperature to obtain the target product.
Example 2
According to the formula CaY1.97Al4SiO120.1682g of CaO and Y are respectively weighed according to the stoichiometric ratio of the elements in 0.03Eu2O3:1.3345g、Al2O3:1.2235g、SiO2:0.3605g、Eu2O30.0317 g. The raw materials are put into an agate mortar, absolute ethyl alcohol is used as a dispersion medium to be fully ground and uniformly mixed, then the mixture is placed into a corundum crucible to be calcined for the first time under the air atmosphere, the calcining temperature is 900 ℃,the calcination time is 4 hours, and the sample is taken out after the sample is naturally cooled to the room temperature. And (3) taking absolute ethyl alcohol as a dispersion medium, grinding and uniformly mixing the mixture after the first calcination, and calcining for the second time in an air atmosphere, wherein the calcining temperature is 1400 ℃, and the calcining time is 5 hours. After the product was cooled to room temperature, the mixture after the second calcination was ground and mixed uniformly with anhydrous ethanol as a dispersion medium, and then placed in a reducing atmosphere (atmosphere composition 5% H)2And +95% Ar) for the third time, wherein the calcining temperature is 800 ℃, and the calcining time is 1 hour, so as to obtain the target product.
Example 3
For CaY1.97Al4SiO12The sintering temperature of 0.03Eu reducing atmosphere is 900 ℃, the sintering time is 1 hour, and the target product can be obtained by the same method as the embodiment 2 under other conditions.
Example 4
For CaY1.97Al4SiO12The sintering temperature of 0.03Eu reducing atmosphere is 1000 ℃, the sintering time is 1 hour, and the target product can be obtained by the same method as the embodiment 2 under the other conditions.
Example 5
For CaY1.97Al4SiO12The sintering temperature of 0.03Eu reducing atmosphere is 1200 ℃, the sintering time is 1 hour, and the target product can be obtained by the same method as the embodiment 2 under the other conditions.
Example 6
For CaY1.97Al4SiO12The sintering temperature of 0.03Eu reducing atmosphere is 1300 ℃, the sintering time is 1 hour, and the target product can be obtained by the same method as the embodiment 2 under other conditions.
Table 1 shows statistics of blue light emission intensity with a main peak at 420 nm and red light emission intensity with a main peak at 615 nm of the phosphor prepared in examples 2-6 provided by the present invention under excitation of ultraviolet light with a wavelength of 275 nm.
Table 1:
as can be seen from FIG. 1, the XRD pattern of the phosphor disclosed by the present invention shows the trend of relative intensity variation and Y3Al5O12The standard map PDF #73-1370 is consistent, which shows that the phosphor prepared by the invention has higher purity. As can be seen from FIG. 2, the phosphor prepared in example 1 emits a typical Eu under excitation of UV light having a wavelength of 254 nm3+615 nm main peak red light; example 2 phosphor prepared by calcining at 800 deg.C for 1 hour in a reducing atmosphere under the same other preparation conditions as in example 1, except for typical Eu3+615 nm main peak of red light emission, Eu also appears2+Blue light emission at 420 nm, with the characteristics of red-blue dual emission. Fig. 3 shows emission spectra of the phosphors prepared in embodiments 2 to 6 under excitation of ultraviolet light of 275 nm, and it can be known from table 1 that, on the premise of calcining for the same time in a reducing atmosphere, the relative emission intensity of fluorescent pink blue dual emission can be adjusted by increasing the calcining temperature, and it is easy to know that the total emission intensity of the phosphors is also further increased along with the increase of the calcining temperature. As can be seen from FIG. 4, with the increase of the excitation wavelength, the emission of the phosphor in the red region will gradually decrease, and the emission in the blue region gradually increases, and the phosphor disclosed by the invention can emit stronger red light under the excitation of ultraviolet light with a wavelength of 230 nm, and can be excited by ultraviolet light with a wavelength of 230-375 nm to generate stronger blue light emission.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A spectrum-adjustable red-blue dual-emission europium-doped aluminate fluorescent powder is characterized in that: the fluorescent powder has the following chemical expression: CaY2-xAl4SiO12xEu, wherein x is 0.001-0.05.
2. A method for preparing the spectrally tunable red-blue dual-emission europium-doped aluminate phosphor of claim 1, which comprises the following steps: comprises the following steps:
(1) using calcium ion-containing compound, yttrium oxide, aluminum oxide, silicon dioxide and europium oxide as raw materials, and adopting chemical expression CaY2-xAl4SiO12Accurately weighing corresponding raw materials according to the stoichiometric ratio of corresponding elements in xEu, wherein the value range of x is 0.001-0.05, and grinding and uniformly mixing the weighed raw materials to obtain a mixture;
(2) calcining the mixture obtained in the step (1) in an air atmosphere at the temperature of 600-950 ℃ for 1-8 hours;
(3) cooling the calcined mixture to room temperature along with the furnace, grinding and uniformly mixing, and calcining in an air atmosphere at the calcining temperature of 1000-1450 ℃ for 1-8 hours;
(4) and cooling the calcined mixture to room temperature along with the furnace, grinding and uniformly mixing, and calcining in a reducing atmosphere at the calcining temperature of 600-1400 ℃ for 0-8 hours to obtain the red-blue dual-emission aluminate fluorescent powder.
3. The method of claim 2, wherein the red-blue dual-emission europium-doped aluminate phosphor with adjustable spectrum is prepared by the following steps: the compound containing calcium ions in the step (1) is one of calcium oxide and calcium carbonate.
4. The method of claim 2, wherein the red-blue dual-emission europium-doped aluminate phosphor with adjustable spectrum is prepared by the following steps: the calcining temperature in the step (2) is 800-900 ℃, and the calcining time is 4-6 hours; the calcining temperature in the step (3) is 1200-1400 ℃, and the calcining time is 4-8 hours; the calcination temperature in the step (4) is 800-1300 ℃, and the calcination time is 1-6 hours.
5. The method of claim 2, wherein the red-blue dual-emission europium-doped aluminate phosphor with adjustable spectrum is prepared by the following steps: and (4) the reducing atmosphere in the step is one of nitrogen-hydrogen mixed gas, argon-hydrogen mixed gas and carbon monoxide gas.
6. The method of claim 2, wherein the red-blue dual-emission europium-doped aluminate phosphor with adjustable spectrum is prepared by the following steps: in the steps (1), (3) and (4), distilled water and/or a volatile organic solvent is added during mixing, wherein the volatile organic solvent is one of ethanol and acetone.
7. The use of the spectrally tunable red-blue dual-emission europium-doped aluminate phosphor of claim 1, wherein: the red-blue dual-emission europium-doped aluminate fluorescent powder is applied to illumination, display and photoluminescence chromaticity adjustment with ultraviolet light of 230-375 nanometers as an excitation source, and emits blue light with a main peak of 420 nanometers and red light with a main peak of 615 nanometers.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113150783A (en) * | 2021-04-27 | 2021-07-23 | 中国科学院长春应用化学研究所 | Color-adjustable afterglow luminescent material, preparation method thereof and lighting product |
| CN115340366A (en) * | 2022-08-12 | 2022-11-15 | 江苏师范大学 | High-color-rendering-index full-spectrum fluorescent material and preparation method thereof |
| CN116333730A (en) * | 2023-03-22 | 2023-06-27 | 河北大学 | Adjustable ultraviolet light and white light dual-emission fluorescent powder and preparation method thereof |
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| CN107868661A (en) * | 2016-09-28 | 2018-04-03 | 中国科学院上海硅酸盐研究所 | A kind of multiband ultraviolet excitation single-matrix white fluorescent material and preparation method thereof |
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| M.S. BHAGAT ET AL.: "Photoluminescence properties of green emitting CaY2Al4SiO12:Tb3+ garnet phosphor", 《OPTIK》 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113150783A (en) * | 2021-04-27 | 2021-07-23 | 中国科学院长春应用化学研究所 | Color-adjustable afterglow luminescent material, preparation method thereof and lighting product |
| CN113150783B (en) * | 2021-04-27 | 2022-11-01 | 中国科学院长春应用化学研究所 | Color-adjustable afterglow luminescent material, preparation method thereof and lighting product |
| CN115340366A (en) * | 2022-08-12 | 2022-11-15 | 江苏师范大学 | High-color-rendering-index full-spectrum fluorescent material and preparation method thereof |
| CN115340366B (en) * | 2022-08-12 | 2024-02-27 | 江苏师范大学 | High-color-rendering-index full-spectrum fluorescent material and preparation method thereof |
| CN116333730A (en) * | 2023-03-22 | 2023-06-27 | 河北大学 | Adjustable ultraviolet light and white light dual-emission fluorescent powder and preparation method thereof |
| CN116333730B (en) * | 2023-03-22 | 2024-01-30 | 河北大学 | Adjustable ultraviolet light and white light dual-emission fluorescent powder and preparation method thereof |
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