CN116333733A - Method for preparing high quantum efficiency ultraviolet emission melem fluorescent powder in ammonia atmosphere - Google Patents
Method for preparing high quantum efficiency ultraviolet emission melem fluorescent powder in ammonia atmosphere Download PDFInfo
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- CN116333733A CN116333733A CN202310313322.0A CN202310313322A CN116333733A CN 116333733 A CN116333733 A CN 116333733A CN 202310313322 A CN202310313322 A CN 202310313322A CN 116333733 A CN116333733 A CN 116333733A
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 63
- YSRVJVDFHZYRPA-UHFFFAOYSA-N melem Chemical compound NC1=NC(N23)=NC(N)=NC2=NC(N)=NC3=N1 YSRVJVDFHZYRPA-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000011161 development Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 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
- 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
- C09K11/0883—Arsenides; Nitrides; Phosphides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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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
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- 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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- Organic Chemistry (AREA)
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- Power Engineering (AREA)
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Abstract
The method for preparing the high quantum efficiency ultraviolet emission melem fluorescent powder in the ammonia atmosphere comprises the following five steps: 1. a certain amount of melamine is weighed as a raw material, the raw material is spread in a 20 mL long-strip alumina crucible boat, and a cover is covered. 2. The crucible boat was placed in a tube furnace. Vacuumizing, and introducing ammonia gas to perform gas washing. And continuously introducing ammonia into the furnace tube after the air in the furnace tube is completely discharged. 3. The tube furnace was opened and the temperature was raised to 400℃where it was calcined at constant temperature for 2 hours. 4. After the calcination is finished, the power supply of the tube furnace is stopped, and the sample is naturally cooled to room temperature. 5. The cooled sample was taken out and placed in an agate mortar and ground to a fine powder. Sieving to obtain the ultraviolet-emitting melem fluorescent powder with high quantum efficiency. The method is simple, the used raw materials are low in price and environment-friendly, the method is expected to be applied to ultraviolet LED devices, the social energy application efficiency can be improved, and the environmental pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of luminescent material preparation, and particularly relates to a method for preparing high quantum efficiency ultraviolet-emitting melem fluorescent powder in an ammonia atmosphere.
Background
In 2021, the "fourteen-five planning" in China indicates that "the resource utilization efficiency is required to be comprehensively improved" and the green economy is greatly developed ". Light Emitting Diodes (LEDs) as a new generation of lighting devices have the advantages of long service life, high energy efficiency, etc. The popularization of LED lighting devices is greatly promoted, and the 'fourteen-five planning' important measure is realized. The fluorescent powder conversion LED lighting device has low cost, simple structure and good reliability, and is a main implementation mode of the current LED lighting device. Among these, the phosphor plays an important role.
Currently, fluorescent powders are mainly composed of rare earth elements. The rare earth fluorescent powder has good stability and luminous performance, and plays an important role in LED illumination. However, rare earth elements are rare in reserves and expensive, and are non-renewable resources. Meanwhile, the exploitation of rare earth resources inevitably causes huge damage to the environment. The development environment is friendly, and the sustainable development of the fluorescent powder is of great significance. Graphite phase carbon nitride (g-C) 3 N 4 ) Is a semiconductor mainly composed of nitrogen element and carbon element, and has certain fluorescence property. g-C 3 N 4 The preparation method is simple, low in cost and good in stability. At the same time, g-C 3 N 4 Does not contain any metal element, has no pollution to the environment and has wide application prospect. However, g-C 3 N 4 The quantum efficiency of the fluorescent powder is lower, and the application requirement of the fluorescent powder cannot be met. Melem as g-C 3 N 4 A stable precursor in the synthesis process has good stability. At the same time, relative to g-C 3 N 4 The quantum efficiency of melem is much higher, and the melem has very wide application prospect as fluorescent powder. However, the synthesis of melem is generally obtained by calcining melamine in air, inevitably with defects in the crystal structure, reducing its fluorescence efficiency. According to the invention, the synthesis atmosphere of melem is changed by means of the tube furnace, melamine is calcined in the ammonia atmosphere, the defect concentration in the melem is reduced, and the quantum efficiency of the melem is further improved. The invention develops the millerThe amine fluorescent powder has the advantages of simple synthesis method, low cost, high quantum efficiency, suitability for development of ultraviolet LED equipment and important research significance.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing high-quantum-efficiency ultraviolet-emitting melem fluorescent powder in an ammonia atmosphere. According to the method, melamine is calcined in an ammonia atmosphere by means of a tube furnace, so that the high-quantum-efficiency melem fluorescent powder is obtained. The fluorescent powder does not contain any metal element, is simple to prepare and low in cost, can further improve the energy utilization efficiency, lightens environmental pollution and promotes sustainable economic development when being applied to ultraviolet LED equipment.
In order to solve the technical problems, the invention adopts the following technical scheme: the method for preparing the high quantum efficiency ultraviolet emission melem fluorescent powder in the ammonia atmosphere comprises the following steps:
step one: a predetermined amount of melamine (C 3 H 6 N 6 99% concentration, analytically pure) as a raw material, tiling the raw material in a 20 mL strip-shaped alumina crucible boat, and covering with a cover;
step two: placing the crucible boat into a tube furnace; pumping the tubular furnace to vacuum by using a vacuum pump, and then introducing ammonia gas into the tubular furnace to reach standard atmospheric pressure;
step three: opening the tube furnace, heating to 400 ℃ at a heating rate of 3 ℃/min, and calcining at the constant temperature for a period of time;
step four: after the calcination is finished, the power supply of the tube furnace is stopped, ammonia gas is kept continuously introduced, and the sample is naturally cooled to room temperature. Stopping ammonia gas input after the temperature of the tube furnace is reduced to a specific temperature;
step five: taking out the cooled sample, placing the sample in an agate mortar, and grinding the sample into fine powder; and (3) sieving the sample in a 200-mesh sieve to obtain the ultraviolet-emitting melem fluorescent powder with high quantum efficiency.
Further, the predetermined amount of melamine in step one was 2.0. 2.0 g.
Further, in the second step, ammonia gas is introduced into the tubular furnace for repeating the process for three times, and gas washing is performed; the ammonia gas injection tube furnace used a constant rate of 0.2 ccm.
Further, in the third step, the constant temperature calcination is carried out for a period of time of 2 h.
Further, the temperature of the tube furnace in the fourth step is reduced to a specific temperature of 20 ℃.
By adopting the technical scheme, compared with other fluorescent materials, the invention calcines melamine in an ammonia atmosphere by virtue of the tube furnace, thereby obtaining the ultraviolet-emitting melem fluorescent powder with high quantum efficiency, and the obtained ultraviolet-emitting melem fluorescent powder has the advantages of high quantum efficiency, no metal, stable performance and the like. The method is simple, the used raw materials are low in price and environment-friendly, the method is expected to be applied to ultraviolet LED devices, the social energy application efficiency can be improved, and the environmental pollution is reduced.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a graph showing the contrast of the illumination of melem synthesized in an ammonia atmosphere and an air atmosphere;
FIG. 3 is a graph of the color of melem synthesized in an ammonia atmosphere versus an air atmosphere;
FIG. 4 is a graph of the quantum efficiency of melem synthesized in an ammonia atmosphere.
Detailed Description
The present invention will be described in detail with reference to the specific embodiments and fig. 1 to 4, but the scope of the present invention is not limited to the following examples, which should be included in the entire contents of the patent application. The size of the high quantum efficiency ultraviolet emission melem fluorescent powder prepared by calcining melamine in the ammonia atmosphere is about 200-2000 nm. The graph (figure 2) of the comparison of the illumination of melem synthesized in ammonia and air demonstrates that the illumination of melem synthesized in ammonia is better than that of melem synthesized in air. The color graph (fig. 3) illustrates that the sample emits mainly bluish-violet light. The quantum efficiency test chart (fig. 4) shows that the quantum efficiency is extremely high. Fig. 1 shows a specific flow of the present invention.
Example 1
Step one: 2.0. 2.0 g Melamine (C) was weighed out using an analytical balance 3 H 6 N 6 99% strength, analytically pure) as a raw material, the raw material was tiled in a 20 mL elongated alumina crucible boat, and covered.
Step two: the crucible boat was placed in a tube furnace. And (3) vacuumizing the furnace tube by using a vacuum pump, and then introducing ammonia gas into the furnace tube to reach the standard atmospheric pressure. The above procedure was repeated three times to perform "scrubbing". After all the air in the furnace tube is discharged, ammonia is continuously introduced into the furnace tube, and the air flow rate is 0.2 cc/min.
Step three: the tube furnace was opened and the heating program was raised to 400℃at a heating rate of 3℃per minute, at which temperature calcination was carried out for 2 hours.
Step four: after the calcination is finished, the power supply of the tube furnace is stopped, ammonia gas is kept continuously introduced, and the sample is naturally cooled to room temperature. After the tube furnace temperature was reduced to a specified temperature, ammonia gas input was stopped.
Step five: the cooled sample was taken out and placed in an agate mortar and ground to a fine powder. And (3) sieving the sample in a 200-mesh sieve to obtain the ultraviolet-emitting melem fluorescent powder with high quantum efficiency.
Example 2
Step one: using an analytical balance, 4.0. 4.0 g melamine (C 3 H 6 N 6 99% strength, analytically pure) as a raw material, the raw material was tiled in a 20 mL elongated alumina crucible boat, and covered.
Step two: the crucible boat was placed in a tube furnace. And (3) vacuumizing the furnace tube by using a vacuum pump, and then introducing ammonia gas into the furnace tube to reach the standard atmospheric pressure. The above procedure was repeated three times to perform "scrubbing". After all the air in the furnace tube is discharged, ammonia is continuously introduced into the furnace tube, and the air flow rate is 0.2 cc/min.
Step three: after the calcination is finished, the power supply of the tube furnace is stopped, ammonia gas is kept continuously introduced, and the sample is naturally cooled to room temperature. After the tube furnace temperature was reduced to a specified temperature, ammonia gas input was stopped.
Step four: after the calcination is finished, the power supply of the tube furnace is stopped, and the sample is naturally cooled to room temperature.
Step five: the cooled sample was taken out and placed in an agate mortar and ground to a fine powder. And (3) sieving the sample in a 200-mesh sieve to obtain the ultraviolet-emitting melem fluorescent powder with high quantum efficiency.
The foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (5)
1. The method for preparing the high quantum efficiency ultraviolet emission melem fluorescent powder in the ammonia atmosphere is characterized by comprising the following steps of: the method comprises the following steps:
step one: a predetermined amount of melamine (C 3 H 6 N 6 99% concentration, analytically pure) as a raw material, tiling the raw material in a 20 mL strip-shaped alumina crucible boat, and covering with a cover;
step two: placing the crucible boat into a tube furnace; pumping the tubular furnace to vacuum by using a vacuum pump, and then introducing ammonia gas into the tubular furnace to reach standard atmospheric pressure;
step three: opening the tube furnace, heating to 400 ℃ at a heating rate of 3 ℃/min, and calcining at the constant temperature for a period of time;
step four: after the calcination is finished, the power supply of the tube furnace is stopped, ammonia gas is kept continuously introduced, the sample is naturally cooled to room temperature,
stopping ammonia gas input after the temperature of the tube furnace is reduced to a specific temperature;
step five: taking out the cooled sample, placing the sample in an agate mortar, and grinding the sample into fine powder; and (3) sieving the sample in a 200-mesh sieve to obtain the ultraviolet-emitting melem fluorescent powder with high quantum efficiency.
2. The method for preparing the high quantum efficiency ultraviolet emission melem fluorescent powder in the ammonia atmosphere according to claim 1, which is characterized in that: the predetermined amount of melamine in step one was 2.0. 2.0 g.
3. The method for preparing the high quantum efficiency ultraviolet emission melem fluorescent powder in the ammonia atmosphere according to claim 1 or 2, which is characterized in that: step two, ammonia gas is introduced into the tubular furnace for repeating the steps three times, and gas washing is carried out; the ammonia gas injection tube furnace used a constant rate of 0.2 ccm.
4. The method for preparing the high quantum efficiency ultraviolet emission melem fluorescent powder in the ammonia atmosphere according to claim 3, wherein the method comprises the following steps of: and in the third step, calcining at constant temperature for a period of time of 2 h.
5. The method for preparing the high quantum efficiency ultraviolet emission melem phosphor in the ammonia atmosphere as claimed in claim 4, wherein the method comprises the following steps: and in the fourth step, the temperature of the tube furnace is reduced to 20 ℃ at a specific temperature.
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CN109294571A (en) * | 2018-12-12 | 2019-02-01 | 临沂大学 | A kind of carbon nitrogen powder yellow fluorescent material and preparation method |
CN114591733A (en) * | 2020-12-03 | 2022-06-07 | 南京大学 | Preparation method of graphite-phase carbon nitride fluorescent powder with controllable fluorescence emission wavelength |
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CN102851027A (en) * | 2012-10-16 | 2013-01-02 | 河北工业大学 | Green environment-friendly method for preparing BCNO fluorescent powder |
CN102874778A (en) * | 2012-10-16 | 2013-01-16 | 河北工业大学 | Method for preparing BCNO fluorescent powder by sintering precursors at low temperature |
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