CN114591733A - Preparation method of graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength - Google Patents
Preparation method of graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength Download PDFInfo
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- CN114591733A CN114591733A CN202011397171.4A CN202011397171A CN114591733A CN 114591733 A CN114591733 A CN 114591733A CN 202011397171 A CN202011397171 A CN 202011397171A CN 114591733 A CN114591733 A CN 114591733A
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- 239000000843 powder Substances 0.000 title claims abstract description 61
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000001338 self-assembly Methods 0.000 claims abstract description 15
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 10
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000007613 environmental effect Effects 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000975 co-precipitation Methods 0.000 claims 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000001354 calcination Methods 0.000 claims 1
- 238000000265 homogenisation Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- JTTIOYHBNXDJOD-UHFFFAOYSA-N 2,4,6-triaminopyrimidine Chemical compound NC1=CC(N)=NC(N)=N1 JTTIOYHBNXDJOD-UHFFFAOYSA-N 0.000 abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052786 argon Inorganic materials 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 9
- HNYOPLTXPVRDBG-UHFFFAOYSA-N barbituric acid Chemical compound O=C1CC(=O)NC(=O)N1 HNYOPLTXPVRDBG-UHFFFAOYSA-N 0.000 description 8
- 125000000714 pyrimidinyl group Chemical group 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000012719 thermal polymerization Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- -1 pyrimidine heterocyclic compound Chemical class 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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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
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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Abstract
The invention discloses a preparation method of graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength, which utilizes an intermolecular hydrogen bond self-assembly technology to prepare cyanuric acid and melamine self-assembly precursors coupled by 2, 4, 6-triaminopyrimidine in different proportions, and the precursors are calcined at high temperature under the protection of argon gas to prepare the pyrimidine-coupled carbon nitride fluorescent powder with controllable fluorescence emission wavelength and the like. The pyrimidine coupled carbon nitride fluorescent powder prepared by the method has the advantages of large specific surface area, simple and efficient preparation, controllable yield and suitability for large-scale production and application. Importantly, the pyrimidine coupled carbon nitride fluorescent powder prepared by the method has the advantages of controllable fluorescence emission wavelength, environmental protection, low cost, good fluorescence performance and the like, and has great development potential in the field of LEDs.
Description
Technical Field
The invention discloses a preparation method of graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength, and relates to the fields of LED fluorescent powder, invisible printing materials and the like.
Technical Field
Currently, Light Emitting Diode (LED) phosphor materials are important materials for next generation light emitting devices. However, the current fluorescent powder has high heavy metal content, large scale production difficulty and high cost, so that the further application of the fluorescent powder in the future is limited. LEDs are the choice of the next generation of lighting devices due to their long lifetime, compact design and significant energy savings. At present, more and more fluorescent powder materials such as perovskite quantum dots, rare earth metal fluorescent powder and the like are used for assembling LEDs, and have the outstanding advantages of low energy consumption, high brightness, high luminous efficiency and the like, so that the fluorescent powder materials are widely developed. However, the fluorescent powder material still has the problems of low storage capacity, high toxicity, poor stability, environmental unfriendliness and the like, so that the further industrialization of the fluorescent powder material is limited.
With the development of novel non-metallic materials, the advantages of unique photoelectric properties, stable chemical properties, simple preparation process, low cost and the like attract wide attention, and the novel non-metallic materials are widely applied to the fields of energy development, device assembly and the like. Based on various advantages of non-metallic materials, the pyrimidine coupled graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength is prepared by the method, has the advantages of excellent fluorescence property, environmental protection, low toxicity, suitability for large-scale preparation and the like, and has important potential in assembly and application of LED devices. In addition, the non-metal fluorescent powder material can emit fluorescent light from green light to red light, the green light and the red light are used as basic hues of the LED, and the preparation of high-quality non-metal fluorescent powder is an important subject of the future white light LED. The fluorescent powder material provided by the method has the characteristics of simple process, environmental friendliness, low cost and the like, and has important potential and value.
Disclosure of Invention
The invention provides a method for preparing graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength by utilizing hydrogen bond self-assembly and high-temperature polymerization.
Specifically, the present invention includes the following:
the graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength is prepared by coupling 2, 4, 6-triaminopyrimidine or barbituric acid serving as a pyrimidine heterocyclic ring with a carbonitrideazine ring, ingeniously preparing a precursor through hydrogen bond self-assembly, and forming the fluorescent powder which is free of metal, easy to disperse and good in fluorescence performance after high-temperature polymerization.
Preferably, the pyrimidine heterocyclic compound used for polymerizing the graphite-phase carbon nitride fluorescent powder is 2, 4, 6-triaminopyrimidine and barbituric acid.
Preferably, the preparation method of the graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength specifically comprises the following steps:
a) the precursor of the pyrimidine ring-coupled carbonitrozine ring is prepared by self-assembly of melamine, cyanuric acid and 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of 2, 4, 6-triaminopyrimidine or 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of barbituric acid hydrogen bond in a molar ratio of 0.5%, 1%, 5%, 10%, 20%, 30%.
b) Filtering the precursor in the step (a) by using a 220nm filter membrane filtering process to obtain white powder;
c) heating the precursor in the step (b) by a thermal polymerization process under the protection of inert gas to obtain light yellow powder;
d) placing the fluorescent powder obtained in the step (c) in an agate ball milling tank for ball milling for 2 hours at 300r/min or dispersing in ethanol for strong ultrasound for 8 hours to prepare graphite-phase carbon nitride fluorescent powder with uniform particles and controllable emission wavelength;
preferably, the step (a) uses 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of 2, 4, 6-triaminopyrimidine or 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of barbituric acid to perform hydrogen bond self-assembly to prepare the precursor.
Preferably, in the step (c), argon is used as a protective gas, 550 ℃ is used as a polymerization temperature, and the reaction is maintained for 4 hours, so that light yellow to orange red powder is prepared.
In the step (d), the sample has better dispersibility by ball milling for 2 hours and ethanol dispersion strong ultrasound for 8 hours, so that uniform fluorescent powder is obtained.
The graphite-phase carbon nitride fluorescent powder with controllable emission wavelength prepared by the invention has larger specific surface area, simple and efficient preparation and controllable yield, is suitable for large-scale production, can control the proportion of pyrimidine ring raw materials in cyanuric acid and melamine self-assembly precursors to control the property of fluorescence, and has the advantages of no metal, no toxicity, environmental protection, good fluorescence property and the like. The fluorescent powder is prepared by a one-step high-temperature calcination method under the protection of argon, has low cost, is suitable for industrial production, and has great development potential in the field of LED optical devices.
Description of the drawings:
FIG. 1 is a flow chart of the preparation of graphite phase carbon nitride phosphor with controllable emission wavelength.
FIG. 2 is a fluorescent substance diagram of the prepared graphite-phase carbon nitride fluorescent powder with controllable emission wavelength under 365nm light excitation.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following embodiments.
As shown in fig. 1, embodiment 1 of the present invention includes:
the preparation process of the graphite phase carbon nitride fluorescent powder with controllable emission wavelength comprises the following steps:
(1) preparation of graphite phase carbon nitride fluorescent powder precursor
1) The preparation method comprises the steps of completely dissolving melamine, cyanuric acid and 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of 2, 4, 6-triaminopyrimidine or 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of barbituric acid in a molar ratio of 0.5%, 1%, 10%, 20%, 30% and 50% in deionized water at 60 ℃, respectively mixing and stirring the 2, 4, 6-triaminopyrimidine and the melamine for 5min, dripping the completely dissolved cyanuric acid into the melamine, carrying out self-assembly through hydrogen bonds, standing for 24h, keeping the temperature at 60 ℃ to obtain white sediment of a precursor of a pyrimidine ring-coupled carbonitrozine ring, and filtering the sediment through a 220nm filter membrane filtration process to obtain white powder;
2) or firstly mixing and stirring cyanuric acid and barbituric acid for 5min, then dripping the completely dissolved melamine into the cyanuric acid, self-assembling through hydrogen bonds, standing for 24h, keeping the temperature at 60 ℃ to obtain a white precipitate of a precursor of the pyrimidine ring-coupled carbonitrozine ring, and filtering the precipitate by a 220nm filter membrane filtration process to obtain white powder;
(2) preparation of graphite phase carbon nitride fluorescent powder
1) The fluorescent powder is prepared by heating the precursor prepared in the step (1) to 550 ℃ by temperature programming (2 ℃/min) under inert gas Ar (99.99 percent, 50mL/min) and preserving the heat for 4 hours to obtain yellowish to orange red powder;
2) putting 50mg of the fluorescent powder obtained by the thermal polymerization in the step 1) in an agate ball milling tank for ball milling for 2h at 300r/min or dispersing in 50mL of ethanol for strong ultrasound for 8h to prepare graphite-phase carbon nitride fluorescent powder with uniform particles;
a) the precursor of the pyrimidine ring-coupled carbonitrozine ring is prepared by self-assembly of melamine, cyanuric acid and 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of 2, 4, 6-triaminopyrimidine or 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of barbituric acid hydrogen bond in a molar ratio of 0.5%, 1%, 5%, 10%, 20%, 30%.
b) Filtering the precursor in the step (a) by using a 220nm filter membrane filtering process to obtain white powder;
c) heating the precursor in the step (b) by a thermal polymerization process under the protection of inert gas to obtain light yellow powder;
d) placing the fluorescent powder obtained in the step (c) in an agate ball milling tank for ball milling for 2 hours at 300r/min or dispersing in ethanol for strong ultrasound for 8 hours to prepare graphite-phase carbon nitride fluorescent powder with uniform particles and controllable emission wavelength;
preferably, the step (a) uses 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of 2, 4, 6-triaminopyrimidine or 0.5%, 1%, 5%, 10%, 20%, 30%, 50% of barbituric acid to perform hydrogen bond self-assembly to prepare the precursor.
Preferably, in the step (c), argon is used as a protective gas, 550 ℃ is used as a polymerization temperature, and the reaction is maintained for 4 hours, so that light yellow to orange red powder is prepared.
In the step (d), the sample has better dispersibility by ball milling for 2 hours and ethanol dispersion strong ultrasound for 8 hours, so that uniform fluorescent powder is obtained.
Claims (8)
1. A carbon nitride fluorescent powder with controllable fluorescence emission wavelength is characterized in that: the carbon nitride fluorescent powder has the advantages of controllable fluorescence emission wavelength, environmental protection, low cost, good fluorescence property, simple and efficient preparation, controllable yield, suitability for large-scale production and the like.
2. The pyrimidine-coupled carbon nitride phosphor according to claim 1, wherein: the pyrimidine coupled carbon nitride fluorescent powder can emit green to red wavelength fluorescence when being excited by 365nm exciting light.
3. A preparation method of pyrimidine coupled carbon nitride fluorescent powder is characterized by comprising the following steps:
a) preparing a precursor of the pyrimidine coupled carbon nitride fluorescent powder by utilizing an intermolecular hydrogen bond self-assembly technology of the three raw materials;
b) standing and filtering the precursor in the step (a) to obtain yellowish powder;
c) calcining the yellow powder obtained in the step (b) at the high temperature of 550 ℃ for 4 hours under the protection of Ar gas;
d) and (c) ball-milling and crushing the sample obtained in the step (c), or performing ultrasonic homogenization in an ethanol solvent for application.
4. The method of claim 3, wherein method one: the precursor of the pyrimidine coupled carbon nitride fluorescent powder prepared by hydrogen bond self-assembly in the step (a) is completely dissolved in water at 60 ℃ by using cyanuric acid and melamine with equal molar quantities as raw materials, 2, 4, 6-triaminopyrimidine heterocyclic conjugates with the molar proportions of 0.5%, 1%, 5%, 10%, 20%, 30%, 50% and the like are added in the self-assembly process, and the precursor is formed by coprecipitation.
5. The method of claim 3, wherein method two: the precursor of the pyrimidine coupled carbon nitride fluorescent powder prepared by hydrogen bond self-assembly in the step (a) is completely dissolved in water at 60 ℃ by using cyanuric acid and melamine with equal molar amounts as raw materials, and barbituric acid pyrimidine heterocyclic conjugates with the molar proportions of 0.5%, 2%, 5%, 10%, 20%, 30%, 50% and the like are added in the self-assembly process and coprecipitated to form the precursor.
6. The method according to claim 3, wherein the precursor of pyrimidine coupled carbon nitride phosphor formed by coprecipitation in step (b) is left standing in a solution at 60 ℃ for 24 hours, filtered, washed and dried to obtain yellowish powder.
7. The method as claimed in claim 3, wherein the step (c) is to calcine the obtained yellowish precursor at 550 ℃ for 4h under the protection of Ar gas with the purity of 99.9% and the programmed temperature of 2 ℃/min to obtain yellowish to orange-red powder.
8. The method of claim 3, wherein the pyrimidine-coupled carbon nitride phosphor in step (d) is ball milled (300r/min, 2h) or the powder is dispersed in ethanol for 8 h; a homogeneous powder was obtained and dispersed in the aqueous solution.
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Cited By (1)
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