CN110129041B - Green nitrogen oxide fluorescent material and manufacturing method thereof - Google Patents
Green nitrogen oxide fluorescent material and manufacturing method thereof Download PDFInfo
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- CN110129041B CN110129041B CN201910351489.XA CN201910351489A CN110129041B CN 110129041 B CN110129041 B CN 110129041B CN 201910351489 A CN201910351489 A CN 201910351489A CN 110129041 B CN110129041 B CN 110129041B
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Abstract
The invention provides a green nitrogen oxide fluorescent material and a manufacturing method thereof, wherein the chemical general formula of the luminescent material is Ba6‑ xEuxSi12O21+0.5yCl3‑yN5Wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3. The green nitrogen oxide fluorescent material manufactured by the manufacturing method has a brand new chemical composition which is Eu2+The luminescent material is an activator, has good thermal quenching property, low raw material cost and relatively low synthesis temperature, can be excited by blue light to emit green light, and thus, the luminescent material is applied to white light LED devices.
Description
Technical Field
The invention relates to a luminescent material, in particular to a green nitrogen oxide fluorescent material and a manufacturing method thereof.
Background
Firstly, LED lighting is currently the most mainstream lighting technology, and has many advantages such as high efficiency, solid structure, energy saving, and small volume. The fluorescent powder is an indispensable material in the LED lighting technology, and various spectrum types including white light can be obtained through the light color conversion of the fluorescent powder.
Second, green light is one of the three primary colors, and the most commercially mature lighting chip product is the blue chip. Therefore, under the excitation of the blue light chip, high-quality white light can be obtained by the light color conversion of the green fluorescent powder and the red fluorescent powder. The current red phosphor is, for example, CaAlSiN3Eu and Sr2Si5N8Eu, etc. And the available and commercialized green phosphor includes Sr2SiO4Eu (patent document 1, Chordachu, Rolingling, pratin, a method for producing Co-doped silicate Green phosphor for led, CN103468250A), Lu3Al5O12Ce (patent document two, T. Sarstel, W. Boolean, P. Schmidt, W. Melel, illumination system comprising a radiation source and a fluorescent material, CN1761835A) and beta-SiAlON: Eu (patent document three, Naoto Hiros)aki, Hideyuki Emoto, Masahiro Ibukiyama, β -Type silicon fluorescent substance, WO2006121083A1), and the like. But Sr2SiO4Eu, Lu, the poor thermal quenching characteristic3Al5O12Ce is high in raw material cost, while the synthesis temperature of beta-SiAlON to Eu exceeds 1850 ℃, which is difficult to be achieved by common equipment.
Finally, nitroxides are important host materials for new fluorescent materials. Many oxynitrides can achieve excellent luminescence properties by doping with rare earth ions, which, although unpredictable, involves creative efforts. However, few publications are available at present based on the mechanism of the chlorine-oxygen-nitrogen compound as a fluorescent material. This is because the chlorine-containing material has a low melting point, and is more volatile during synthesis, which makes it difficult to control the final composition and luminescence properties of the material.
Disclosure of Invention
Therefore, the first purpose of the invention is to provide a green oxynitride fluorescent material. The material is Eu2+The luminescent material is an activator, has good thermal quenching property, low raw material cost and relatively low synthesis temperature, can be excited by blue light to emit green light, and thus, the luminescent material is applied to white light LED devices.
In order to achieve the purpose, the invention adopts the following technical scheme:
a green oxynitride fluorescent material has a chemical formula as follows:
Ba6-xEuxSi12O21+0.5yCl3-yN5
wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3.
Preferably, x may be 0.24 and y may be 2.
The second purpose of the invention is to provide a method for manufacturing a green oxynitride fluorescent material. The manufacturing method comprises the following steps:
A) mixing a Ba precursor, a Eu precursor, a Si precursor, a Cl precursor and an N precursor, and carrying out high-temperature high-pressure solid-phase reaction under the atmosphere of nitrogen to obtain an intermediate;
B) and mixing the intermediate, the Ba precursor, the Si precursor and the N precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the green nitrogen oxide fluorescent material.
Preferably, in step a), the molar ratio of Ba, Eu, Si, Cl and N in the Ba precursor, Eu precursor, Si precursor, Cl precursor and N precursor is (4-x): x: 2: (3-y): 1, the chemical formula of the obtained intermediate is as follows: ba4-xEuxSi2O5+ 0.5yCl3-yN, wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3.
Preferably, in step B), the intermediate, Ba precursor, Si precursor and N precursor are mixed in a molar ratio of 1: 2: 10: 4.
preferably, in step A), the Ba precursor is selected from the group consisting of carbonates of Ba, oxides of Ba, oxalates of Ba, BaCl2And nitrate of Ba, wherein BaCl2Is necessary; the Eu precursor may be selected from at least one of a carbonate of Eu, an oxide of Eu, an oxalate of Eu, and a nitrate of Eu; cl precursor from BaCl2(ii) a The Si precursor is selected from silicon dioxide and silicon nitride; the N precursor is from silicon nitride.
Preferably, in the step B), the Ba precursor is selected from at least one of a carbonate of Ba, an oxide of Ba, an oxalate of Ba, and a nitrate of Ba; the Si precursor is selected from silicon dioxide and silicon nitride; the N precursor is from silicon nitride.
Preferably, the purity of the Ba precursor, the Eu precursor, the Si precursor, the Cl precursor and the N precursor is not lower than 99.5%.
Preferably, in the step A), the temperature of the high-temperature high-pressure solid-phase reaction is 1000-1200 ℃, the atmosphere is nitrogen, the pressure is 0.5-1 MPa, and the time of the high-temperature high-pressure solid-phase reaction is 4-10 h.
Preferably, in the step B), the reducing atmosphere is ammonia gas or a nitrogen-hydrogen mixed gas; the temperature of the high-temperature solid phase is 1500-1700 ℃, and the time of the high-temperature solid phase is 4-10 h.
Advantageous effects
Compared with the prior artIn contrast, the green oxynitride fluorescent material manufactured according to the method of the present invention has a completely new chemical composition, with Eu2+The luminescent material is an activator, has good thermal quenching property, low raw material cost and relatively low synthesis temperature, can be excited by blue light to emit green light, and thus, the luminescent material is applied to white light LED devices. The chemical composition of the luminescent material is Ba6-xEuxSi12O21+0.5yCl3-yN5Wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3.
Drawings
FIG. 1 is a graph showing an emission spectrum of a luminescent material obtained in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
The application provides a green nitrogen oxide fluorescent material, which has a chemical general formula as follows:
Ba6-xEuxSi12O21+0.5yCl3-yN5
wherein 0 < x < 0.5, 0 < y < 3, preferably 0.1 < x < 0.4, 1.5 < y < 2.5, more preferably 0.2 < x < 0.3, 1.8 < y < 2.2. In one embodiment of the present application, x is preferably 0.01, and y is preferably 0.01; in one embodiment of the present application, x is preferably 0.05, and y is preferably 0.5; in one embodiment of the present application, x is preferably 0.24, and y is preferably 2; in one embodiment of the present application, x is preferably 0.3, and y is preferably 2.1; in another embodiment of the present application, x is preferably 0.4 and y is preferably 2.5.
The application provides a method for manufacturing the green nitric oxide fluorescent material, which comprises the following steps:
A) mixing a Ba precursor, a Eu precursor, a Si precursor, a Cl precursor and an N precursor, and carrying out high-temperature high-pressure solid-phase reaction under the atmosphere of nitrogen to obtain an intermediate;
B) and mixing the intermediate, the Ba precursor, the Si precursor and the N precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the green nitrogen oxide fluorescent material.
In the step a), the molar ratio of Ba, Eu, Si, Cl and N in the Ba precursor, Eu precursor, Si precursor, Cl precursor and N precursor is (4-x): x: 2: (3-y): 1, the chemical formula of the obtained intermediate is as follows: ba4-xEuxSi2O5+0.5yCl3-yN, wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3.
In the step a), the Ba precursor may be a compound containing Ba well known in the art, and is not particularly limited, and in the present invention, it is preferable that the Ba precursor is selected from the group consisting of carbonate of Ba, oxide of Ba, oxalate of Ba, BaCl2And nitrate of Ba, wherein BaCl2Is essential, more preferably a carbonate of Ba (i.e., barium carbonate) and BaCl2(ii) a The Eu precursor may be selected from at least one of a carbonate of Eu, an oxide of Eu, an oxalate of Eu, and a nitrate of Eu, and is more preferably an oxide of Eu, i.e., europium oxide; cl precursor from BaCl2(ii) a The Si precursor is selected from silicon dioxide and silicon nitride; the N precursor is from silicon nitride.
In the step B), the intermediate, the Ba precursor, the Si precursor and the N precursor are mixed, wherein the molar ratio of the intermediate, Ba, Si and N is 1: 2: 10: 4.
in the step B), the Ba precursor may be a compound containing Ba well known in the art, and is not particularly limited, and in the present invention, the Ba precursor is preferably at least one selected from the group consisting of a carbonate of Ba, an oxide of Ba, an oxalate of Ba, and a nitrate of Ba, and more preferably barium carbonate; the Si precursor is selected from silicon dioxide and silicon nitride; the N precursor is derived from silicon nitride.
The purity of the Ba precursor, the Eu precursor, the Si precursor, the Cl precursor and the N precursor is not lower than 99.5%, and the higher the purity is, the less impurities are in the obtained luminescent material.
In the step A), the temperature of the high-temperature high-pressure solid-phase reaction is 1000-1200 ℃, the atmosphere is nitrogen, the pressure is 0.5-1 MPa, and the time of the high-temperature high-pressure solid-phase reaction is 4-10 h.
In the step B), the reducing atmosphere is ammonia gas or nitrogen-hydrogen mixed gas; the temperature of the high-temperature solid phase is 1500-1700 ℃, and the time of the high-temperature solid phase is 4-10 h.
The temperature of the high-temperature high-pressure solid phase in the step A) is preferably 1000-1200 ℃, the atmosphere is nitrogen, and the pressure is 0.5-1 MPa; in one embodiment of the present invention, the temperature of the high temperature solid phase is preferably 1100 ℃, and the pressure is 0.8 MPa.
The time for high-temperature and high-pressure solid phase in the step A) is preferably 4-10 h, and more preferably 5-8 h; in some embodiments provided herein, the time for the high temperature solid phase is preferably 6 hours.
The temperature of the high-temperature solid phase in the step B) is preferably 1500-1700 ℃; in some embodiments provided herein, the temperature of the high temperature solid phase is preferably 1600 ℃.
The time for high-temperature solid phase in the step B) is preferably 4-10 h, and more preferably 5-8 h; in some embodiments provided herein, the time for the high temperature solid phase is preferably 6 hours.
The reducing atmosphere in the step B) is a dry atmosphere known to those skilled in the art, and is not particularly limited, and ammonia gas is preferred in the present invention;
the high-temperature (high-pressure) solid reaction phase is preferably carried out in a high-temperature furnace; after the reaction of the step A) and the step B) is carried out in sequence, the reaction product is cooled to room temperature along with the furnace, and the green nitrogen oxide fluorescent material can be obtained.
The embodiment of the application successfully manufactures the green nitrogen oxide fluorescent material by adopting a high-temperature (high-pressure) solid-phase reaction.
In order to further illustrate the present invention, the following describes a green oxynitride fluorescent material and a method for manufacturing the same in detail with reference to examples.
The reagents used in the following comparative examples and examples are all commercially available.
Comparative example 1
The raw material is SrCO3(analytically pure), Eu2O3(analytically pure) and SiO2(analytically pure) at a molar ratio of 1.96: 0.02: 1, grinding and mixing the above raw materials, placing into a crucible, sintering at 1500 deg.C for 6h in a high temperature furnace under ammonia reducing atmosphere, and performing vacuum distillationCooling the furnace to room temperature to obtain Sr as a theoretical chemical component1.96Eu0.04SiO4The light-emitting material of (1).
The fluorescent material obtained in comparative example 1 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 525nm, and the highest intensity of the spectral luminescence peak at room temperature and the highest intensity of the spectral luminescence peak at 150 ℃ (i.e. thermal quenching characteristic) are shown in table 1. It can be seen that comparative example 1 has poor thermal quenching characteristics corresponding to the fluorescent material, and the luminous intensity is only 10% of that at room temperature at 150 deg.C
Example 1
The raw material is BaCl2(analytically pure), BaCO3(analytically pure), Eu2O3(analytically pure), Si3N4(analytically pure) and SiO2(analytical grade), molar ratio 1.495: 2.495: 0.005: 0.25: 1.25, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture for 6 hours at 1100 ℃ in a high-temperature furnace under the nitrogen pressure of 0.8MPa, and cooling the mixture to room temperature along with the furnace to obtain Ba as a theoretical chemical component3.99Eu0.01Si2O5.005Cl2.99An intermediate of N. The intermediate, BaCO3(analytically pure), SiO2(analytically pure) and Si3N4(analytical purity) in a molar ratio of 1: 2: 10: 4, grinding and uniformly mixing the materials, putting the materials into a crucible, sintering the materials for 6 hours at 1600 ℃ in a high-temperature furnace in an ammonia reducing atmosphere, and cooling the materials to room temperature along with the furnace to obtain the green nitric oxide fluorescent material with the chemical component of Ba5.99Eu0.01Si12O21.005Cl2.99N5。
The fluorescent material obtained in example 1 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 1. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 528nm, and the highest intensity of the spectral luminescence peak at room temperature and the highest intensity of the spectral luminescence peak at 150 ℃ (i.e. thermal quenching characteristic) are shown in table 1. It can be seen that example 1 is superior to comparative example 1 in thermal quenching characteristics of the fluorescent material, and the luminous intensity at 150 ℃ is 92% of that at room temperature.
Example 2
The raw material is BaCl2(analytically pure), BaCO3(analytically pure), Eu2O3(analytically pure), Si3N4(analytically pure) and SiO2(analytical grade), molar ratio 1.25: 2.7: 0.025: 0.25: 1.25, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture for 6 hours at 1100 ℃ in a high-temperature furnace under the nitrogen pressure of 0.8MPa, and cooling the mixture to room temperature along with the furnace to obtain Ba as a theoretical chemical component3.95Eu0.05Si2O5.25Cl2.5An intermediate of N. The intermediate, BaCO3(analytically pure), SiO2(analytically pure) and Si3N4(analytical purity) in a molar ratio of 1: 2: 10: 4, grinding and uniformly mixing the materials, putting the materials into a crucible, sintering the materials for 6 hours at 1600 ℃ in a high-temperature furnace in an ammonia reducing atmosphere, and cooling the materials to room temperature along with the furnace to obtain the green nitric oxide fluorescent material with the chemical component of Ba5.95Eu0.05Si12O21.25Cl2.5N5。
The fluorescent material obtained in example 2 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 529nm, and the highest intensity of the spectral luminescence peak at room temperature and the highest intensity of the spectral luminescence peak at 150 ℃ (i.e. thermal quenching characteristic) are shown in table 1. It can be seen that example 2 is superior to comparative example 1 in thermal quenching characteristics of the fluorescent material, and the luminous intensity at 150 ℃ is 93% of that at room temperature.
Example 3
The raw material is BaCl2(analytically pure), BaCO3(analytically pure), Eu2O3(analytically pure), Si3N4(analytically pure) and SiO2(analytical grade), molar ratio 0.5: 3.26: 0.12: 0.25: 1.25, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture for 6 hours at 1100 ℃ in a high-temperature furnace under the nitrogen pressure of 0.8MPa, and cooling the mixture to room temperature along with the furnace to obtain Ba as a theoretical chemical component3.76Eu0.24Si2O6Intermediates of ClN. The intermediate, BaCO3(analytically pure), SiO2(analytically pure) and Si3N4(analytical purity) in a molar ratio of 1: 2: 10: 4, grinding and uniformly mixing the materials, putting the materials into a crucible, sintering the materials for 6 hours at 1600 ℃ in a high-temperature furnace in an ammonia reducing atmosphere, and cooling the materials to room temperature along with the furnace to obtain the green nitric oxide fluorescent material with the chemical component of Ba5.76Eu0.24Si12O22ClN5。
The fluorescent material obtained in example 3 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 532nm, and the highest intensity of the spectral luminescence peak at room temperature and the highest intensity of the spectral luminescence peak at 150 ℃ (i.e. thermal quenching characteristic) are shown in table 1. It can be seen that the fluorescent material of example 3 has better thermal quenching characteristics than the fluorescent material of comparative example 1, and the luminous intensity at 150 ℃ is 91% of that at room temperature.
Example 4
The raw material is BaCl2(analytically pure), BaCO3(analytically pure), Eu2O3(analytically pure), Si3N4(analytically pure) and SiO2(analytical grade), molar ratio 0.45: 3.25: 0.15: 0.25: 1.25, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture for 6 hours at 1100 ℃ in a high-temperature furnace under the nitrogen pressure of 0.8MPa, and cooling the mixture to room temperature along with the furnace to obtain Ba as a theoretical chemical component3.7Eu0.3Si2O6.05Cl0.9An intermediate of N. The intermediate, BaCO3(analytically pure), SiO2(analytically pure) and Si3N4(analytical purity) in a molar ratio of 1: 2: 10: 4, grinding and uniformly mixing the materials, putting the materials into a crucible, sintering the materials for 6 hours at 1600 ℃ in a high-temperature furnace in an ammonia reducing atmosphere, and cooling the materials to room temperature along with the furnace to obtain the green nitric oxide fluorescent material with the chemical component of Ba5.7Eu0.3Si12O22.05Cl0.9N5。
The fluorescent material obtained in example 4 was analyzed by a fluorescence spectrometer. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 530nm, and the highest intensity of the spectral luminescence peak at room temperature and the highest intensity of the spectral luminescence peak at 150 ℃ (i.e. thermal quenching characteristic) are shown in table 1. It can be seen that the fluorescent material of example 4 has better thermal quenching characteristics than the fluorescent material of comparative example 1, and the luminous intensity at 150 ℃ is 90% of that at room temperature.
Example 5
The raw material is BaCl2(analytically pure), BaCO3(analytically pure), Eu2O3(analytically pure), Si3N4(analytically pure) and SiO2(analytical grade), molar ratio 0.25: 3.15: 0.2: 0.25: 1.25, grinding and uniformly mixing the raw materials, putting the mixture into a crucible, sintering the mixture for 6 hours at 1100 ℃ in a high-temperature furnace under the nitrogen pressure of 0.8MPa, and cooling the mixture to room temperature along with the furnace to obtain Ba as a theoretical chemical component3.6Eu0.4Si2O6.25Cl0.5An intermediate of N. The intermediate, BaCO3(analytically pure), SiO2(analytically pure) and Si3N4(analytical purity) in a molar ratio of 1: 2: 10: 4, grinding and uniformly mixing the materials, putting the materials into a crucible, sintering the materials for 6 hours at 1600 ℃ in a high-temperature furnace in an ammonia reducing atmosphere, and cooling the materials to room temperature along with the furnace to obtain the green nitric oxide fluorescent material with the chemical component of Ba5.6Eu0.4Si12O22.25Cl0.5N5。
The fluorescent material obtained in example 1 was analyzed by a fluorescence spectrometer to obtain an emission spectrum thereof, as shown in fig. 1. It can be seen that the material can be excited by blue light, the main peak of the emission spectrum is located near 528nm, and the highest intensity of the spectral luminescence peak at room temperature and the highest intensity of the spectral luminescence peak at 150 ℃ (i.e. thermal quenching characteristic) are shown in table 1. It can be seen that example 5 is superior to comparative example 1 in thermal quenching characteristics of the fluorescent material, and the luminous intensity at 150 ℃ is 94% of that at room temperature.
Table 1
The above examples are only for illustrating the embodiments of the present invention and illustrating the technical features of the present invention, and are not intended to limit the scope of the present invention. Any modification or equivalent arrangement which can be easily implemented by a person skilled in the art is intended to be within the scope of the present invention, which is defined by the following claims.
Claims (10)
1. A green oxynitride fluorescent material is characterized in that the chemical general formula of the fluorescent material is as follows: ba6- xEuxSi12O21+0.5yCl3-yN5，
Wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3.
2. The green oxynitride fluorescent material of claim 1, wherein x is 0.24 and y is 2.
3. The method for manufacturing a green oxynitride fluorescent material according to any one of claims 1 to 2, comprising the steps of:
A) mixing a Ba precursor, a Eu precursor, a Si precursor, a Cl precursor and an N precursor, and carrying out high-temperature high-pressure solid-phase reaction under the atmosphere of nitrogen to obtain an intermediate;
B) and mixing the intermediate, the Ba precursor, the Si precursor and the N precursor, and carrying out high-temperature solid-phase reaction in a reducing atmosphere to obtain the green nitrogen oxide fluorescent material.
4. The method of claim 3, wherein in step A), the molar ratio of Ba, Eu, Si, Cl, and N in the Ba precursor, the Eu precursor, the Si precursor, the Cl precursor, and the N precursor is (4-x): x: 2: (3-y): 1, the chemical formula of the obtained intermediate is as follows: ba4-xEuxSi2O5+0.5yCl3-yN, wherein x is more than 0 and less than 0.5, and y is more than 0 and less than 3.
5. The method for manufacturing a green oxynitride fluorescent material of claim 3, wherein in the step B), the molar ratio of the intermediate, Ba precursor, Si precursor and N precursor is 1: 2: 10: 4.
6. The method of claim 3, wherein the purity of the Ba precursor, the Eu precursor, the Si precursor, the Cl precursor, and the N precursor is not less than 99.5%.
7. The method for preparing a green oxynitride fluorescent material according to claim 3, wherein in the step A), the temperature of the high-temperature high-pressure solid-phase reaction is 1000 to 1200 ℃, the atmosphere is nitrogen, the pressure is 0.5 to 1MPa, and the time of the high-temperature high-pressure solid-phase reaction is 4 to 10 hours.
8. The method according to claim 3, wherein in step B), the reducing atmosphere is ammonia gas or a mixed gas of nitrogen and hydrogen; the temperature of the high-temperature solid phase is 1500-1700 ℃, and the time of the high-temperature solid phase is 4-10 h.
9. The method of claim 3, wherein in the step A), the Ba precursor is selected from the group consisting of Ba carbonate, Ba oxide, Ba oxalate, BaCl2And nitrate of Ba, wherein BaCl2Is necessary; the Eu precursor may be selected from at least one of a carbonate of Eu, an oxide of Eu, an oxalate of Eu, and a nitrate of Eu; the Cl precursor is from BaCl2(ii) a The Si precursor is selected from silicon dioxide and silicon nitride; the N precursor is from silicon nitride.
10. The method of claim 3, wherein in the step B), the Ba precursor is selected from at least one of a carbonate of Ba, an oxide of Ba, an oxalate of Ba, and a nitrate of Ba; the Si precursor is selected from silicon dioxide and silicon nitride; the N precursor is from silicon nitride.
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