CN113999671A - Fluorescent powder for lighting display white light LED and preparation and application thereof - Google Patents
Fluorescent powder for lighting display white light LED and preparation and application thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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- C09K11/7733—Halogenides with alkali or alkaline earth metals
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/77342—Silicates
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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 discloses fluorescent powder for a lighting display white light LED and preparation and application thereof. The chemical general formula of the fluorescent powder is Sr1‑x‑yMyBaSiO4‑yFy:xEu2+(M is Na or K). Weighing the raw materials according to the stoichiometric ratio of the chemical general formula; mixing and grinding; placing the mixture in an alumina crucible, preserving heat in a reducing atmosphere at a high temperature, cooling to room temperature, grinding and sintering the product, and sieving to obtain the fluorescent powder for the illumination display white light LED. The fluorescent powder is used in various lighting display devices using near ultraviolet light as an excitation source. The fluorescent powder solves the key problems of poor thermal stability when a near ultraviolet chip excites the tricolor fluorescent powder to form white light in the prior art, and the core problems of low light conversion and energy conversion efficiency, poor luminous uniformity, poor color rendering property caused by the lack of green light and the like caused by poor thermal stability, and is suitable for various illumination displays taking near ultraviolet light as an excitation sourceIn the piece.
Description
Technical Field
The invention belongs to the technical field of rare earth luminescent materials, relates to fluorescent powder for a white light LED in illumination display, and discloses green fluorescent powder capable of being excited by near ultraviolet; the invention also relates to a preparation method and application of the green fluorescent powder.
Background
The fluorescent powder white light LED has the advantages of high energy efficiency, long service life, compact structure, environmental friendliness and the like, and is a fourth-generation novel lighting and display light source developed after incandescent lamps, fluorescent lamps and high-pressure gas discharge lamps. The fluorescent powder can strongly absorb the blue light or near ultraviolet light emitted by the LED chip and effectively re-emit the blue light or near ultraviolet light in red, green or yellow regions of a visible spectrum, and the whole device can emit white light by combining the fluorescent powder with different colors. In the application of white light LED lighting, a combination of blue LED chip and yellow phosphor is mainly used industrially and commercially, but the white light LED with the combination has a problem of incomplete spectrum, so that the color rendering effect is poor. In order to further improve the color development effect of white light LED illumination, a combination of three kinds of fluorescent powder of near ultraviolet LED chips and red, green and blue is generated, the combination basically can cover the spectrum of the whole visible light region, and the color development effect is good. However, if the emission intensity of some of the phosphors is reduced for some reason, the brightness and color rendering effect of the whole white LED device are reduced. Furthermore, the human eye is particularly sensitive to the green region of the visible spectrum, and if the green portion of the white light is attenuated or missing, the illumination or display effect is greatly compromised. Therefore, the green phosphor plays a crucial role in illuminating or displaying white light quality. The thermal stability is an important index for judging the luminescent performance of the fluorescent powder. Generally, the luminous intensity of the phosphor decreases with increasing temperature, and this effect is a thermal quenching effect. Since white light or green light for illumination or display cannot be deteriorated due to the decrease in emission intensity of the green phosphor, the green phosphor used in the white LED must have good thermal stability.
The rare earth doped alkaline earth metal orthosilicate fluorescent powder is an important luminescent material, has more than forty years of research history, and has good luminescent properties, such as adjustable excitation and emission peaks, high luminescent intensity, rich luminescent colors, high quantum efficiency and the like; and the fluorescent powder has stable chemical properties, simple preparation process and low manufacturing cost, and is a good choice for the fluorescent powder for the white light LED. Commercial green phosphor SrBaSiO4: Eu2+Has strong absorption in the near ultraviolet to blue region and strong luminous intensity, but has low thermal stabilityThe performance of the white light LED device is difficult to meet the practical application requirements of the white light LED device, and the white light LED device gradually exits the market at present. Therefore, it is of great theoretical and practical significance to develop a fluorescent powder for a high-efficiency white light LED that solves the above-mentioned problems.
Disclosure of Invention
The invention aims to provide the green fluorescent powder for the illumination display white light LED, which improves the thermal stability of the fluorescent powder and meets the application requirement of high-performance devices.
The invention also aims to provide a preparation method of the green fluorescent powder.
The third purpose of the invention is to provide the application of the green fluorescent powder in white light LEDs for lighting display.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a green fluorescent powder for white LED with illumination and display has a chemical general formula of Sr1-x-yMyBaSiO4-yFy: xEu2+Wherein x is more than or equal to 0.01 and less than or equal to 0.20, y is more than or equal to 0.05 and less than or equal to 0.5, and M is Na or K.
The other technical scheme adopted by the invention is as follows: the preparation method of the green fluorescent powder comprises the following steps:
1) according to the chemical formula Sr1-x-yMyBaSiO4-yFy: xEu2+The raw materials are respectively weighed according to the stoichiometric ratio, wherein,
sr is introduced via carbonate, oxide, hydroxide, nitrate, sulfate or phosphate;
ba is introduced via carbonate, oxide, hydroxide, nitrate, sulfate or phosphate;
eu is introduced through carbonate, oxide, hydroxide, nitrate, sulfate or phosphate;
si is introduced through oxide;
na is introduced via fluoride, oxide, hydroxide, carbonate, nitrate, sulfate or phosphate; or K is introduced via fluoride, oxide, hydroxide, carbonate, nitrate, sulphate or phosphate;
fully mixing all the taken raw materials to form a mixture, and grinding to obtain a mixed material;
2) placing the mixed material in an alumina crucible, heating to 900-1100 ℃ under normal pressure in a reducing atmosphere, preserving heat for 0-2 h, then heating to 1000-1600 ℃, preserving heat for 1-10 h, and cooling to room temperature along with a furnace to obtain a sintered product;
3) and grinding and sieving the sintered product to obtain the green fluorescent powder for the white light LED for illumination display.
The reducing atmosphere consists of 5% nitrogen and 95% hydrogen by volume.
The third technical scheme adopted by the invention is as follows: the application of the aluminum fluorescent powder in various lighting display devices using near ultraviolet light as an excitation source. The near ultraviolet light excitation source comprises a near ultraviolet LED chip.
The fluorescent powder is prepared by adopting a high-temperature solid phase method, belongs to an alkaline earth metal orthosilicate system, has the advantages of good crystallinity, strong luminous brightness, high luminous efficiency, stable physicochemical properties and the like, and is particularly prepared by Na+、K+After cation regulation and control, the material has good thermal stability; the fluorescent material has strong light absorption at 350-450 nm of near ultraviolet light, the peak value of an excitation peak is about 410nm, the fluorescent material can be effectively excited by a near ultraviolet chip, green fluorescence can be emitted under the excitation of the near ultraviolet light, and the peak value of the emission peak is adjustable at 510-530 nm; the fluorescent powder has very good contribution to white light in a white light LED for illumination display, because when the blue light, the red light and the green light are combined to obtain white light, the green light with the emission peak near 520 nm can obtain very bright white light, and meanwhile, the green light with the emission peak between 510 and 530 nm can show clearer and more vivid green light components in the combination of the blue light, the green light and the red light, so that the fluorescent powder is suitable for various illumination display devices taking near ultraviolet light as an excitation source.
The fluorescent powder solves the problems caused by thermal stability in the prior art, namely the problem of low thermal stability of the existing alkaline earth metal orthosilicate system fluorescent powder, and the key problems of low light conversion and energy conversion efficiency, poor luminous uniformity, poor color rendering property caused by green light deficiency and the like caused by low thermal stability. The preparation method of the fluorescent powder is simple, easy to operate, high in controllability, stable in performance and easy for industrial production.
Drawings
FIG. 1 is a comparison of the XRD pattern and the standard pattern of the phosphor prepared in example 1.
FIG. 2 shows the excitation spectrum and the emission spectrum of the phosphor prepared in example 1.
FIG. 3 is a graph showing the change of the emission spectrum with temperature of the phosphor obtained in example 1.
FIG. 4 shows the phosphor prepared in example 1 and SrBaSiO in the prior art4Temperature quenching curve of the fluorescent powder is compared.
FIG. 5 shows the XRD pattern and the standard pattern of the phosphor prepared in example 2.
FIG. 6 shows the excitation spectrum and the emission spectrum of the phosphor prepared in example 2.
FIG. 7 shows the phosphor prepared in example 2 and SrBaSiO in the prior art4Temperature quenching curve of the fluorescent powder is compared.
FIG. 8 shows the XRD pattern and the standard pattern of the phosphor prepared in example 3.
FIG. 9 shows the excitation spectrum and the emission spectrum of the phosphor obtained in example 3.
FIG. 10 shows the phosphor prepared in example 3 and SrBaSiO in the prior art4Temperature quenching curve of the fluorescent powder is compared.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
According to the chemical formula Sr0.68Na0.3BaSiO3.7F0.3: 0.02Eu2+The stoichiometric ratio of the raw materials is respectively called SrCO3、BaCO3、SiO2、Eu2O3And NaF, and mixing the taken raw materials to form a mixture. Grinding, mixing, placing in an alumina crucible, placing in a high temperature tubular furnace, heating to 1000 deg.C under mixed atmosphere of nitrogen and hydrogen at normal pressure for 1 hr, heating to 1400 deg.C, firing for 4 hr, cooling to room temperature, grindingAnd sieving to obtain the green fluorescent powder for the white light LED for illumination display.
FIG. 1 shows the XRD pattern and standard pattern (ICSD-7653) of the phosphor prepared in example 1. As can be seen from FIG. 1, the XRD pattern of the phosphor prepared in example 1 is similar to that of standard SrBaSiO4The XRD pattern (ICSD-7653) of the compound is well consistent, no impurity peak appears, and the substitute ion Na is shown+Successfully enter a host crystal lattice, namely the synthesized fluorescent powder is single-phase and has higher purity.
FIG. 2 is an excitation spectrum and an emission spectrum of the phosphor obtained in example 1. The monitoring wavelength of the excitation spectrum in fig. 2 is 521 nm, and it can be seen that the phosphor powder prepared in example 1 can be excited by ultraviolet light to blue light in a wavelength range of 350 to 450 nm, the excitation spectrum is a wide spectrum, and covers a region from ultraviolet light to blue light, an excitation peak is located near 410nm, and a spectrum peak is high, which indicates that the phosphor powder prepared in the invention can be effectively excited by a near ultraviolet chip; in the emission spectrum of FIG. 2, the excitation wavelength is 410nm and the emission peak is Eu2+The emission peak value of the fluorescent powder is near 521 nm, which shows that the prepared fluorescent powder is suitable for being used as green fluorescent powder for near ultraviolet excited white light LEDs for lighting and displaying.
The emission spectrum of the phosphor prepared in example 1 is plotted as a function of temperature, as shown in FIG. 3. It can be seen that the luminescence intensity of the phosphor decreases with increasing temperature, and the decrease of the luminescence intensity before 150 ℃ is smaller than that after.
Example 1 phosphor prepared in accordance with the prior art and the phosphors SrBaSiO Eu2+As compared to the temperature quenching curve of fig. 4. As can be seen from the figure, the fluorescence quenching performance of the phosphor prepared in example 1 is between 25 ℃ and 125 ℃ and the phosphor SrBaSiO4: Eu2+The difference is not large; the temperature is higher than (including) 125 ℃, and the fluorescence quenching performance of the fluorescent powder prepared in the example 1 is obviously superior to that of the fluorescent powder SrBaSiO in the prior art4: Eu2+The quenching property of (1). Therefore, in the combination of the near ultraviolet LED chip and the blue-green-red fluorescent powder, the green fluorescent powder prepared by the invention is obviously superior to SrBaSiO in the prior art4: Eu2+The fluorescent powder effectively reduces the green light caused by the heat generation of the LED deviceThe quality of the white light is degraded.
Example 2
According to the chemical formula Sr0.78Na0.2BaSiO3.8F0.2: 0.02Eu2+The stoichiometric ratio of the raw materials is respectively called SrCO3、BaCO3、SiO2、Eu2O3And NaF, mixing the obtained raw materials, fully grinding and uniformly mixing the raw materials, placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature tube furnace, heating the mixture to 1000 ℃ under normal pressure and in a mixed atmosphere of nitrogen and hydrogen for 1 hour, heating the mixture to 1400 ℃ for firing for 4 hours, cooling the mixture to room temperature along with the furnace, grinding and sieving the mixture to obtain the green fluorescent powder for the white light LED for lighting display.
FIG. 5 shows the XRD pattern and standard pattern (ICSD-7653) of the phosphor prepared in example 2. from FIG. 5, it can be seen that the XRD pattern of the phosphor prepared in example 2 is similar to that of standard SrBaSiO4The XRD pattern (ICSD-7653) of the compound is well consistent, no impurity peak appears, and the substitute ion Na is shown+Successfully enter a host crystal lattice, namely the fluorescent powder synthesized in the embodiment 2 is single-phase and has higher purity.
FIG. 6 is an excitation spectrum and an emission spectrum of the phosphor obtained in example 2. The monitoring wavelength of the excitation spectrum in fig. 6 is 519 nm, and it can be seen that the phosphor prepared in example 2 can be excited by ultraviolet light to blue light in a wavelength range of 350 to 450 nm, the excitation spectrum is a wide spectrum, an area from ultraviolet light to blue light is covered, an excitation peak is located near 410nm, and a spectrum peak is high, which indicates that the phosphor prepared in example 2 can be effectively excited by a near ultraviolet chip; in the emission spectrum of FIG. 6, the excitation wavelength is 410nm and the emission peak is Eu2+The emission peak of (1) is near 519 nm, which shows that the fluorescent powder prepared in example 2 is suitable for being used as green fluorescent powder for near ultraviolet excited white light LEDs for lighting and displaying.
Example 2 phosphor prepared with prior art Sr0.98BaSiO4:0.02Eu2+The temperature quenching curves of the phosphors are compared, as shown in FIG. 7. It can be seen that the luminescent intensity of the phosphor prepared in example 2 decreases with increasing temperature between 25 ℃ and 200 ℃, and the fluorescence quenching performance is 150 DEG CObviously better than the prior SrBaSiO at the temperature of 200 DEG C4: Eu2+And (3) fluorescent powder.
Example 3
According to the chemical formula Sr0.88Na0.1BaSiO3.9F0.1: 0.02Eu2+The stoichiometric ratio of the raw materials is respectively called SrCO3、BaCO3、SiO2、Eu2O3And NaF, mixing the raw materials, fully grinding and uniformly mixing, placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature tube furnace, heating the mixture to 1000 ℃ under normal pressure and in a mixed atmosphere of nitrogen and hydrogen for heat preservation for 1 hour, heating the mixture to 1400 ℃ for firing for 4 hours, cooling the mixture to room temperature along with the furnace, grinding and sieving the mixture to obtain the green fluorescent powder for the white light LED for lighting display.
FIG. 8 shows the XRD pattern and standard pattern (ICSD-7653) of the phosphor prepared in example 3. from FIG. 8, the XRD pattern and standard SrBaSiO of the phosphor prepared in example 3 can be seen4The XRD pattern (ICSD-7653) of the compound is well consistent, no impurity peak appears, and the substitute ion Na is shown+Successfully enter a host crystal lattice, namely the fluorescent powder synthesized in the embodiment 3 is single-phase and has higher purity.
The excitation spectrum and emission spectrum of the phosphor prepared in example 3 are shown in fig. 9. The monitoring wavelength of the excitation spectrum in fig. 9 is 520 nm, and it can be seen that the phosphor prepared in example 3 can be excited by ultraviolet light to blue light in a wavelength range of 350 to 450 nm, the excitation spectrum is a wide spectrum, which covers a region from ultraviolet light to blue light, the excitation peak is located near 410nm, and the peak value of the spectrum is high, which indicates that the phosphor prepared in example 3 can be effectively excited by the near-ultraviolet chip. FIG. 9 shows an emission spectrum with an excitation wavelength of 410nm and an emission peak of Eu2+The emission peak of (1) is near 520 nm, which shows that the phosphor prepared in example 3 is suitable for being used as green phosphor for near ultraviolet excited white light LED for illumination and display.
Phosphor prepared in example 3 and SrBaSiO phosphor of the prior art4:0.02Eu2+FIG. 10 is a graph comparing the temperature quenching curves of (A). It can be seen that the luminescent intensity of the phosphor prepared in example 3 is increased with temperature between 25 ℃ and 200 DEG CHigh and reduced fluorescence quenching performance at 150-200 deg.C, obviously superior to that of available SrBaSiO4: Eu2+And (3) fluorescent powder.
Example 4
According to the chemical formula Sr0.78K0.2BaSiO3.8F0.2: 0.02Eu2+Respectively weighing SrO and Ba (NO) according to the stoichiometric ratio of the raw materials3)2、SiO2、Eu2(CO3)3、 K2CO3And NH4And F, mixing the raw materials, fully grinding and uniformly mixing, placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature tube furnace, heating the mixture to 1000 ℃ under normal pressure and in a mixed atmosphere of nitrogen and hydrogen for 1 hour, heating the mixture to 1400 ℃ for firing for 4 hours, cooling the mixture to room temperature along with the furnace, grinding and sieving the mixture to obtain the green fluorescent powder for the white light LED for illumination display.
The phosphor prepared in example 4 is a good single phase with high purity; can be effectively excited by near ultraviolet light and blue light of 350 nm to 450 nm, and emits green light with the peak wavelength of 518 nm, and the half-peak width of emission is 67 nm; the thermal stability is still obviously superior to that of the fluorescent powder SrBaSiO in the prior art4: Eu2+。
Example 5
According to the chemical formula Sr0.94K0.05BaSiO3.95F0.05: 0.01Eu2+The stoichiometric ratio of the raw materials is respectively called SrCO3、BaCO3、SiO2、Eu2O3And KF, mixing the raw materials, fully grinding and uniformly mixing, placing the mixture in an alumina crucible, placing the alumina crucible in a high-temperature tube furnace, heating to 1600 ℃ at normal pressure in a mixed atmosphere of nitrogen and hydrogen for heat preservation for 6 hours, heating to 1200 ℃ for firing for 20 hours, cooling to room temperature along with the furnace, grinding and sieving to prepare the green fluorescent powder for the white light LED for illumination display.
Example 6
According to the chemical formula Sr0.3K0.5BaSiO3.5F0.5: 0.2Eu2+The stoichiometric ratio of the raw materials is respectively called SrCO3、BaCO3、SiO2、Eu2O3And KF, mixing the raw materials to form a mixture. Fully grinding and uniformly mixing, placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature tube furnace, heating the mixture to 1300 ℃ for 10 hours under the atmosphere of nitrogen and hydrogen, heating the mixture to 1600 ℃ for firing for 11 hours, cooling the mixture to room temperature along with the furnace, grinding and sieving the mixture to obtain the green fluorescent powder for the white light LED for lighting display.
Example 7
According to the chemical formula Sr0.62K0.28BaSiO3.72F0.28: 0.1Eu2+The stoichiometric ratio of the raw materials is respectively called SrCO3、BaCO3、SiO2、Eu2O3And KF, mixing the raw materials to form a mixture. Fully grinding and uniformly mixing, placing the mixture into an alumina crucible, placing the alumina crucible into a high-temperature tube furnace, heating the mixture to 1000 ℃ for heat preservation for 1 hour under the atmosphere of nitrogen and hydrogen, heating the mixture to 1600 ℃ for firing for 11 hours, cooling the mixture to room temperature along with the furnace, grinding and sieving the mixture to obtain the green fluorescent powder for the white light LED for lighting display.
Claims (5)
1. The fluorescent powder for the white light LED for illumination and display is characterized in that the chemical general formula of the fluorescent powder is Sr1-x- yMyBaSiO4-yFy: xEu2+Wherein x is more than or equal to 0.01 and less than or equal to 0.20, y is more than or equal to 0.05 and less than or equal to 0.5, and M is Na or K.
2. The preparation method of the fluorescent powder for the white light LED for illumination and display as claimed in claim 1, which is characterized by comprising the following steps:
1) according to the chemical formula Sr1-x-yMyBaSiO4-yFy: xEu2+In the stoichiometric ratio of (1), wherein M is Na or K, respectively weighing each raw material,
sr is introduced via carbonate, oxide, hydroxide, nitrate, sulfate or phosphate;
ba is introduced via carbonate, oxide, hydroxide, nitrate, sulfate or phosphate;
eu is introduced through carbonate, oxide, hydroxide, nitrate, sulfate or phosphate;
si is introduced through oxide;
na is introduced by fluoride, oxide, hydroxide, carbonate, nitrate, sulfate, phosphate, or the like; alternatively, K is introduced by fluoride, oxide, hydroxide, carbonate, nitrate, sulfate, phosphate, or the like;
fully mixing all the materials, and grinding to obtain a mixed material;
2) placing the mixed material in an alumina crucible, heating to 900-1100 ℃ under normal pressure in a reducing atmosphere, preserving heat for 0-2 h, then heating to 1200-1600 ℃, preserving heat for 2-20 h, and cooling to room temperature along with a furnace to obtain a sintered product;
3) and grinding and sieving the sintered product to obtain the green fluorescent powder for the illumination display white light LED.
3. The method for preparing fluorescent powder for white LED lighting display according to claim 2, wherein the reducing atmosphere in step 2) is a mixed gas of nitrogen and hydrogen.
4. The method of claim 3, wherein the mixture gas comprises 5% nitrogen and 95% hydrogen by volume.
5. The use of the phosphor for white light LED for illumination display according to claim 1 in various illumination display devices using near ultraviolet light as an excitation source.
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Cited By (1)
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| CN116285962A (en) * | 2023-02-27 | 2023-06-23 | 兰州大学 | Eu (Eu) 2+ Activated chlorine-containing silicate long afterglow material and preparation method and application thereof |
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