CN114702958B - Heat-stable nitrogen oxide fluorescent powder and preparation method and application thereof - Google Patents
Heat-stable nitrogen oxide fluorescent powder and preparation method and application thereof Download PDFInfo
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- CN114702958B CN114702958B CN202210249411.9A CN202210249411A CN114702958B CN 114702958 B CN114702958 B CN 114702958B CN 202210249411 A CN202210249411 A CN 202210249411A CN 114702958 B CN114702958 B CN 114702958B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—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
- C09K11/77348—Silicon Aluminium Nitrides or Silicon Aluminium Oxynitrides
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/0883—Arsenides; Nitrides; Phosphides
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- H—ELECTRICITY
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- H01L33/00—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
- 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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- H01L33/502—Wavelength conversion materials
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Abstract
The invention provides a thermostable nitrogen oxide fluorescent powder, a preparation method and application thereof, belonging to the field of fluorescent powderIn the field of fluorescent materials. The chemical formula of the heat stable nitrogen oxide fluorescent powder is Sr 1‑ x Eu x Al 2 Si 3 ON 6 Wherein 0 is<x is less than or equal to 0.2. The oxynitride of the invention has the advantages of both oxide and nitride, and is prepared by Eu 2+ The doping can realize that yellow light and orange light with the wavelength of 400-700nm can be emitted under the excitation of 365nm near ultraviolet light. Meanwhile, the fluorescent powder provided by the invention has good thermal stability, and can keep the emission intensity of 99.6% at room temperature at most at the working temperature of the LED of about 150 ℃ with almost no loss. The preparation method is simple and feasible, does not need high-pressure conditions, and is suitable for large-scale industrial production and popularization and application.
Description
Technical Field
The invention belongs to the field of fluorescent materials, and particularly relates to a thermally stable nitrogen oxide fluorescent powder and a preparation method and application thereof.
Background
The white light LED lamp has the advantages of long service life, high energy saving, environmental protection and the like, and is a novel illumination and display light source developed after an incandescent lamp, a fluorescent lamp and a high-pressure gas discharge lamp. At present, a combination of a blue light LED chip, yellow fluorescent powder and red fluorescent powder is mainly used in white light LED illumination, and the principle is that part of blue light is absorbed by the fluorescent powder, and the rest of blue light is mixed with light emitted by the yellow fluorescent powder to obtain white light. The method for obtaining the white light has low cost, but the obtained white light has cool color and low color rendering index (lower than 80). In order to further improve the color development effect of white light LED illumination, a scheme uses a combination of near ultraviolet LED chips, blue, green, yellow, red and other fluorescent powder. However, the fluorescent powder is a key point for determining the luminous efficiency, the cooling and heating color and the service life of the LED lamp in any scheme.
Long wavelength visible light (yellow/orange/red) phosphors can be classified into oxides, nitrides, oxynitrides, sulfides, fluorides, and the like. Wherein the sulfides and fluorides have poor chemical stability, the sulfides are easily oxidized and deteriorated, the fluorides are afraid of water and humid environment, and H is involved in the synthesis and use of the sulfides and oxides 2 S, HF and other toxic substances. Typically, the operating temperature of the LED device is about 150 ℃, and at this temperature, the fluorescence thermal quenching phenomenon of the oxide material is serious, and the fluorescence efficiency is obviously reduced due to heating.In contrast, nitrides have a three-position compact structure and have strong heat resistance, but the synthesis conditions of nitrides are severe, and high temperatures (. Gtoreq.1800 ℃) and high pressures (. Gtoreq.8 atm) are generally required. Therefore, it is significant to develop a phosphor that is heat resistant and has relatively mild synthesis conditions.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a thermally stable nitrogen oxide fluorescent powder as well as a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a heat stable nitrogen oxide fluorescent powder, the chemical formula of which is Sr 1-x Eu x Al 2 Si 3 ON 6 Wherein 0 is<x≤0.2。
The oxynitride of the invention has the advantages of both oxide and nitride, and is prepared by Eu 2+ The doping can realize that yellow light and orange light with the wavelength of 400-700nm can be emitted under the excitation of 365nm near ultraviolet light. The inventors have found that, by research, different Eu 2+ The emission spectrum and the emission peak position of the fluorescent powder prepared under the doping amount can be changed correspondingly. Meanwhile, sr prepared under different doping amounts 1- x Eu x Al 2 Si 3 ON 6 The phosphors have different thermal stability but perform better than oxide thermal quenching. Compared with the traditional nitride, the invention has good thermal stability, and simultaneously has lower synthesis temperature without high pressure condition, thereby being suitable for large-scale industrial production and popularization and application.
As a preferred embodiment of the present invention, the phosphor has the chemical formula Sr 1-x Eu x Al 2 Si 3 ON 6 Wherein x is more than or equal to 0.01 and less than or equal to 0.075.
The inventors have found that, when Eu 2+ When the doping amount of the doped fluorescent powder is within the range that x is more than or equal to 0.01 and less than or equal to 0.075, the thermal stability of the fluorescent powder is good, the thermal quenching integral intensity is more than 70% at 150 ℃, and the luminous integral intensity is more than 70%.
As a more preferable embodiment of the invention, the chemical formula of the fluorescent powder is Sr 1-x Eu x Al 2 Si 3 ON 6 Wherein x is more than or equal to 0.01 and less than or equal to 0.025. The inventors have found that, when Eu 2+ When the doping amount of the doped material is within the range of 0.01-0.025, the doped material has good luminous intensity and thermal stability, the thermal quenching integral intensity is more than 86% at 150 ℃, and the luminous integral intensity is more than 70%.
As a preferred embodiment of the present invention, the phosphor has the chemical formula Sr 1-x Eu x Al 2 Si 3 ON 6 Where x=0.01.
The inventors have found that, when Eu 2+ When the doping amount is x=0.01, the thermal stability of the fluorescent powder is optimal, and the thermal quenching integral intensity is more than 99% at 150 ℃ and basically no attenuation exists.
As a preferred embodiment of the present invention, the phosphor has the chemical formula Sr 1-x Eu x Al 2 Si 3 ON 6 Where x=0.025.
The inventors have found that, when Eu 2+ When the doping amount of the doping is x=0.025, the luminous intensity of the fluorescent powder is optimal, and meanwhile, the intensity of the fluorescent powder still keeps 90.2% at the working temperature of the LED at 150 ℃, and the fluorescent powder has good luminous intensity and stability.
As a preferred embodiment of the invention, the fluorescent powder emits yellow and orange light with the wavelength of 400-700nm under the excitation of 365nm near ultraviolet light.
As a preferred embodiment of the present invention, the phosphor has an integrated thermal quenching intensity of greater than 70% at 150 ℃.
As a preferred embodiment of the present invention, the phosphor has a thermal quenching integrated intensity of greater than 99% at 150 ℃.
A preparation method of a thermally stable nitrogen oxide fluorescent powder comprises the following steps:
(1) Weighing the reaction raw materials according to the mole ratio of Sr, eu, al and Si in the chemical formula of the fluorescent powder, and uniformly mixing to obtain a mixture;
(2) Calcining the mixture obtained in the step (1) for 2-6 hours at the temperature of 1500-1700 ℃ in inert atmosphere, and cooling, crushing and grinding sequentially to obtain the fluorescent powder.
As a preferred embodiment of the present invention, in the step (1), the strontium source in the reaction raw material comprises SrCO 3 And SrO; the aluminum source in the reaction raw material comprises any one of simple substance Al and AlN; the silicon source in the reaction raw material comprises simple substances Si and Si 3 N 4 Any one of them; the europium source in the reaction raw material comprises Eu 2 O 3 。
As a preferred embodiment of the present invention, in step (2), the inert atmosphere includes nitrogen and hydrogen; the volume percentage of hydrogen in the inert atmosphere is 2-20%.
As a more preferred embodiment of the present invention, in step (2), the inert atmosphere includes nitrogen and hydrogen; the volume percentage of hydrogen in the inert atmosphere is 10%.
As a preferred embodiment of the present invention, in step (2), the mixture is calcined at a temperature of 1600 ℃ for 4 hours.
The invention also provides application of the heat-stable nitrogen oxide fluorescent powder in an LED device.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention provides a novel Eu 2+ Doped with oxynitride fluorescent powder, the fluorescent powder emits yellow and orange light with the wavelength of 400-700nm under the excitation of 365nm near ultraviolet light.
(2) The fluorescent powder disclosed by the invention has excellent thermal stability, and the optimal components still keep the emission intensity of 99.6% of room temperature at the working temperature of about 150 ℃ of an LED, so that almost no loss is caused.
(3) The preparation method is simple and feasible, does not need high-pressure conditions, and is suitable for large-scale industrial production and popularization and application.
Drawings
FIG. 1 is a graph comparing XRD of the phosphor of example 1 of the present invention with a standard spectrum.
FIG. 2 is a graph showing the excitation and emission spectra of the phosphor of example 1 of the present invention.
FIG. 3 is a graph showing the thermal quenching characteristics of the phosphor of example 1 of the present invention.
FIG. 4 is a graph comparing XRD of the phosphor of example 2 of the present invention with a standard spectrum.
FIG. 5 is a graph showing the excitation and emission spectra of the phosphor of example 2 of the present invention.
FIG. 6 is a graph showing the thermal quenching characteristics of the phosphor of example 2 of the present invention.
FIG. 7 is a graph comparing XRD of the phosphor of example 3 of the present invention with a standard spectrum.
FIG. 8 is a graph showing the excitation and emission spectra of the phosphor of example 3 of the present invention.
FIG. 9 is a graph showing the thermal quenching of the phosphor of example 3 of the present invention.
FIG. 10 is a graph comparing XRD of the phosphor of example 4 of the present invention with a standard spectrum.
FIG. 11 is a graph showing the excitation and emission spectra of the phosphor of example 4 of the present invention.
FIG. 12 is a graph showing the thermal quenching characteristics of the phosphor of example 4 of the present invention.
FIG. 13 is a graph showing the relationship between Eu ion content and luminescence intensity in the phosphor powders of examples 1 to 4 according to the present invention.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. The experimental methods described in the examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available unless otherwise specified.
Example 1
As Sr of the invention 0.99 Eu 0.01 Al 2 Si 3 ON 6 An embodiment of a method for preparing a thermally stable nitrogen oxide phosphor specifically comprises the following steps:
(1) 0.7308g SrCO is accurately weighed according to the proportion 3 、0.0088g Eu 2 O 3 0.4099g AlN and 0.7014g Si 3 N 4 Adding into a mortar, and stirring thoroughly to mix well.
(2) The mixed raw materials were transferred to a 40mL corundum crucible. Placing the crucible into an atmosphere furnace, calcining at 1600 ℃ for 4 hours, and introducing H 2 /N 2 Atmosphere (H) 2 5% of the ratio, N 2 95% of the total weight). And taking out the sample after the temperature in the hearth is reduced to below 200 ℃ for grinding, and crushing to obtain powder.
It was found by testing that a pure phase structured phosphor was obtained, the XRD of which is shown in FIG. 1. The excitation and emission spectra of the fluorescent powder are shown in figure 2, and the fluorescent powder is suitable for excitation of 365nm near ultraviolet light chips, and emits broad-peak yellow light with the peak value of 561nm and covering 400-700 nm. The thermal quenching integral intensity of the fluorescent powder prepared in example 1 is shown in fig. 3 as a function of temperature. The fluorescent powder has good luminescence thermal quenching performance, and still maintains 99.6% of intensity at the working temperature of the LED of 150 ℃, namely has optimal thermal stability when x=0.01.
Example 2
As Sr of the invention 0.975 Eu 0.025 Al 2 Si 3 ON 6 An embodiment of a method for preparing a thermally stable nitrogen oxide phosphor specifically comprises the following steps:
(1) 0.7197g SrCO is accurately weighed according to the proportion 3 、0.0220g Eu 2 O 3 0.4099g AlN and 0.7014g Si 3 N 4 Adding into a mortar, and stirring thoroughly to mix well.
(2) The mixed raw materials were transferred to a 40mL corundum crucible. Placing the crucible into an atmosphere furnace, calcining at 1600 ℃ for 4 hours, and introducing H 2 /N 2 Atmosphere (H) 2 5% of the ratio, N 2 95% of the total weight). And taking out the sample after the temperature in the hearth is reduced to below 200 ℃ for grinding, and crushing to obtain powder. It was found by testing that a pure phase structured phosphor was obtained, the XRD of which is shown in FIG. 4. The excitation and emission spectra of the fluorescent powder are shown in fig. 5, and the fluorescent powder is suitable for excitation of 365nm near ultraviolet light chips, and emits broad-peak yellow light with the peak value of 578nm and covering 400-700 nm.
The thermal quenching integral intensity of the phosphor prepared in example 2 is shown in fig. 6 as a function of temperature. The fluorescent powder has good luminescence thermal quenching performance, and the intensity of the fluorescent powder is still kept at 90.2% at the working temperature of 150 ℃.
Example 3
As Sr of the invention 0.925 Eu 0.075 Al 2 Si 3 ON 6 An embodiment of a method for preparing a thermally stable nitrogen oxide phosphor specifically comprises the following steps:
(1) 0.6828g SrCO is accurately weighed according to the proportion 3 、0.0660g Eu 2 O 3 0.4099g AlN and 0.7014g Si 3 N 4 Adding into a mortar, and stirring thoroughly to mix well.
(2) The mixed raw materials were transferred to a 40mL corundum crucible. Placing the crucible into an atmosphere furnace, calcining at 1600 ℃ for 4 hours, and introducing H 2 /N 2 Atmosphere (H) 2 5% of the ratio, N 2 95% of the total weight). And taking out the sample after the temperature in the hearth is reduced to below 200 ℃ for grinding, and crushing to obtain powder. It was found by the test that a pure phase structured phosphor was obtained, the XRD of which is shown in FIG. 7. The excitation and emission spectra of the fluorescent powder are shown in fig. 8, and the fluorescent powder is suitable for excitation of 365nm near ultraviolet chips, and emits broad-peak yellow light with a peak value of 596nm and covering 400-750 nm.
The thermal quenching integral intensity of the phosphor prepared in example 3 is shown in fig. 9 as a function of temperature. The fluorescent powder has good luminescence thermal quenching performance, and the intensity of 86.2 percent is still maintained at the working temperature of 150 ℃ of the LED.
Example 4
As Sr of the invention 0.800 Eu 0.200 Al 2 Si 3 ON 6 An embodiment of a method for preparing a thermally stable nitrogen oxide phosphor specifically comprises the following steps:
(1) 0.5905g SrCO is accurately weighed according to the proportion 3 、0.1760g Eu 2 O 3 0.4099g AlN and 0.7014g Si 3 N 4 Adding into a mortar, and stirring thoroughly to mix well.
(2) The mixed raw materials were transferred to a 40mL corundum crucible. Placing the crucible into an atmosphere furnace, calcining at 1600 ℃ for 4 hours, and introducing H 2 /N 2 Atmosphere (H) 2 5% of the ratio, N 2 95% of the total weight). And taking out the sample after the temperature in the hearth is reduced to below 200 ℃ for grinding, and crushing to obtain powder. It was found by the test that a pure phase structured phosphor was obtained, the XRD of which is shown in FIG. 10. The excitation and emission spectra of the phosphor are shown in FIG. 11, which shows that the phosphor is suitable for 365nm near ultravioletThe optical chip is excited to emit broad-peak yellow light with the peak value of 614nm and the coverage of 400-750 nm.
The thermal quenching integrated intensity of the phosphor prepared in example 4 is shown in fig. 12 as a function of temperature. The fluorescent powder has good luminescence thermal quenching performance, and the intensity of the fluorescent powder is still kept at 71.3% at the working temperature of 150 ℃ of the LED.
Comparative example 1
As a comparative example of the preparation method of the thermally stable nitrogen oxide phosphor of the present invention, comparative example 1 was added 0.7396g SrCO except for the step (1) 3 And no Eu addition 2 O 3 Other preparation methods and conditions were exactly the same, except for example 1. Tests show that the prepared powder does not have luminescence property due to no Eu doping.
The inventors further studied Eu ion content (chemical formula Sr 1-x Eu x Al 2 Si 3 ON 6 The range of x) and the luminous intensity are shown in fig. 13. Studies have shown Sr 1-x Eu x Al 2 Si 3 ON 6 In the system, when x is more than or equal to 0.01 and less than or equal to 0.075, the fluorescent powder has high luminous intensity and good thermal stability. At x=0.01, the thermal stability of the phosphor is optimal, and the integrated thermal quenching intensity is greater than 99% at 150 ℃, without substantial attenuation. When x=0.025 has the highest luminous intensity, while still maintaining 90.2% of the intensity at the LED operating temperature of 150 ℃.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. A heat stable nitrogen oxide fluorescent powder is characterized in that the chemical formula of the fluorescent powder is Sr 1-x Eu x Al 2 Si 3 ON 6 Wherein x=0.025;
the preparation method of the fluorescent powder comprises the following steps:
(1) Weighing the reaction raw materials according to the mole ratio of Sr, eu, al and Si in the chemical formula of the fluorescent powder, and uniformly mixing to obtain a mixture;
(2) Calcining the mixture obtained in the step (1) for 2-6 hours at the temperature of 1500-1700 ℃ in an inert atmosphere, and sequentially cooling, crushing and grinding to obtain the fluorescent powder.
2. The phosphor of claim 1, wherein the phosphor emits a yellow or orange light of 400-700nm upon excitation by 365nm near ultraviolet light.
3. The phosphor of any of claims 1-2, wherein the phosphor has an integrated thermal quenching intensity of greater than 70% at 150 ℃.
4. The method for preparing the fluorescent powder according to claim 1, comprising the steps of:
(1) Weighing the reaction raw materials according to the mole ratio of Sr, eu, al and Si in the chemical formula of the fluorescent powder, and uniformly mixing to obtain a mixture;
(2) Calcining the mixture obtained in the step (1) for 2-6 hours at the temperature of 1500-1700 ℃ in an inert atmosphere, and sequentially cooling, crushing and grinding to obtain the fluorescent powder.
5. The method according to claim 4, wherein in the step (1), the strontium source in the reaction raw material comprises SrCO 3 And SrO; the aluminum source in the reaction raw material comprises any one of simple substance Al and AlN; the silicon source in the reaction raw material comprises simple substances Si and Si 3 N 4 Any one of them; the europium source in the reaction raw material comprises Eu 2 O 3 。
6. The method of claim 4, wherein in step (2), the inert atmosphere comprises nitrogen and hydrogen; the volume percentage of hydrogen in the inert atmosphere is 2-20%.
7. The process of claim 4, wherein in step (2), the mixture is calcined at a temperature of 1600 ℃ for 4 hours.
8. Use of the phosphor of any one of claims 1-3 in LED devices.
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| KR101163902B1 (en) * | 2010-08-10 | 2012-07-09 | 엘지이노텍 주식회사 | Light emitting device |
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