CN103086332A - Carbon nitride compound fluorescent powder and preparation method thereof - Google Patents
Carbon nitride compound fluorescent powder and preparation method thereof Download PDFInfo
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- CN103086332A CN103086332A CN2013100360074A CN201310036007A CN103086332A CN 103086332 A CN103086332 A CN 103086332A CN 2013100360074 A CN2013100360074 A CN 2013100360074A CN 201310036007 A CN201310036007 A CN 201310036007A CN 103086332 A CN103086332 A CN 103086332A
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Abstract
The invention discloses a preparation method of carbon nitride compound fluorescent powder. The preparation method comprises the following steps of: burning melamine for 2-6h in N2 atmosphere at certain temperature from 300 DEG C to 650 DEG C, and cooling the melamine along with the cooling of the furnace to obtain the carbon nitride compound fluorescent powder having tunable luminescence. With increment of burning temperature, a red shift of a luminescent center of the prepared luminescent material and a luminescent region constantly occurs, and under excitation of wavelength light of 280nm, tunable luminescence of the luminescent center within 400-510nm is generated, and the luminescent region covers emissions of ultraviolet ray, blue light, green light and yellow light, and spreads to a red light region. The invention further discloses carbon nitride compound fluorescent powder prepared by the method, wherein expression general formula of the fluorescent powder is g-C3N4, and the fluorescent powder belongs to a graphite laminated structure. The carbon nitride compound fluorescent powder prepared by the invention plays an important role in illumination and display applications.
Description
Technical field
The present invention relates to luminescent material, particularly a kind of carboritride fluorescent material and preparation method thereof.
Background technology
Day in 1993 Asia (Nichia) company takes the lead in adopting blue light gallium nitride light-emitting diode+gold-tinted fluorescent material YAG:Ce combination to make white light LEDs, its current consumption is only 1/8 of incandescent light, 1/2 of fluorescent lamp can reach 100,000 hours (being about 10 times of luminescent lamps) work-ing life.Just have the remarkable advantages such as high light efficiency, long lifetime, energy-conserving and environment-protective due to white light LEDs, it will progressively replace the incandescent light of power consumption and the luminescent lamp of mercury pollution, become the lighting source of new generation of 21 century.The research of white light LEDs at present remains the field of an awfully hot door.Realize white light LEDs mainly by way of the Multiple Quantum Well type is arranged, polychrome is combined and these three kinds of modes of fluorescent conversion type.Because having, fluorescent conversion type makes simple, the advantages such as cost is low, technology maturation and easy industrialization.At present, the most of blue-ray LED+YAG:Ce method that adopts of white light LEDs on market.This " blue chip+bloom " product is during as lighting source, because ruddiness composition in YAG:Ce fluorescent material emmission spectrum is few, press blue-ray LED+YAG:Ce phosphor combination scheme color developing when the low color temperature white light LED of realizing lower than 4000K relatively poor, undue sombre on visual sense feeling; During as liquid crystal backlight, show that colour gamut is narrow, full-color effect is bad.In order to obtain warm-toned white light LEDs, usually need to add another long wavelength's fluorescent material, as red fluorescence powder.
Nitride is because having obvious electronic cloud expansion effect, abundant structure and stronger covalency, thereby higher in ultraviolet-blue light region assimilated efficiency, and more obvious advantage is being arranged aspect thermostability and chemical stability, in addition, external famous illumination company, as Osram, Philips, GE, day inferior chemistry, Matsushita Electric Industries, Toyota synthesize, Mitsubishi Chemical, Sharp etc. and domestic Beijing space utmost point, grind rare earth, Tong Shida novel material etc. all at the active development Nitride phosphor, and progressively begin to use the white light LEDs product based on Nitride phosphor.
Since current, comparatively popular about the research of Nitride phosphor.But Nitride phosphor is mainly the fluorescent material of rear-earth-doped and doped transition metal ions at present, such light-emitting phosphor excellent performance.As Eu
2+The nitride light-emitting better performances of doping, quantum yield is higher, is luminescent material preferably, but the higher temperature and pressure of synthetic needs of such luminescent material, for the reaction equipment requirements higher, and rare earth ion and the transition metal ion price more expensive, manufacturing cost is higher.And carboritride is synthetic comparatively easy, and material itself is nontoxic, and light-emitting zone has been contained ultraviolet, blue light, and green glow and yellow emission, and be extended between red light district.Significant to white light LEDs.
Summary of the invention
For the above-mentioned shortcoming and deficiency that overcomes prior art, the object of the present invention is to provide a kind of preparation method of carboritride fluorescent material, raw material cheaply is easy to get, and operation is simple.
The carboritride fluorescent material that another object of the present invention is to provide the preparation method of above-mentioned carboritride fluorescent material to obtain.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of carboritride fluorescent material comprises the following steps:
With trimeric cyanamide calcination under nitrogen atmosphere, calcination temperature is 300 ℃-650 ℃, and calcination time is 2-6h, obtains carboritride fluorescent material after furnace cooling.
Described with trimeric cyanamide calcination under nitrogen atmosphere, be specially:
With the trimeric cyanamide alumina crucible of packing into, the silica tube burner hearth calcination of alumina crucible being put into atmosphere furnace stablely in the silica tube burner hearth in the calcination process passes into the N that flow is 75-150sccm
2Air-flow.
After the calcination end of processing, be down to 100 ℃ when the temperature of silica tube burner hearth, close N
2Air-flow.
The carboritride fluorescent material that the preparation method of above-mentioned carboritride fluorescent material obtains, it expresses general formula is g-C
3N
4, be the graphite laminate structure.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) preparation method of carboritride fluorescent material of the present invention, raw material is cheap, be easy to get, and temperature of reaction is lower, and operation is simple.
(2) the present invention can by controlling different calcination temperatures, obtain the different fluorescent material of luminous peak position, along with the rising of calcination temperature, the continuous red shift of emission band, tunable light-emitting zone has been contained ultraviolet, blue light, green glow and yellow emission, and be extended between red light district.
Description of drawings
Fig. 1 is the powder x-ray diffraction spectrum of the sample (1) of embodiments of the invention.
Fig. 2 is the emmission spectrum (λ of sample (1) ~ (8) of embodiments of the invention
ex=280nm).
Fig. 3 is sample (5), (9) of embodiments of the invention, the emmission spectrum (λ of (10)
ex=280nm).
Fig. 4 is the excitation spectrum of the sample (7) of embodiments of the invention.
Fig. 5 is sample (1), (4) of embodiments of the invention, the fluorescence decay curve (λ of (8)
ex=280nm, λ
em=480nm).
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment
Take the trimeric cyanamide (C of 10 parts of 2g
3H
6N
6), the alumina crucible that to be respectively charged into 10 volumes be 20mL carries out respectively 10 experiments, and process is as follows: crucible is put into the silica tube burner hearth of atmosphere furnace, passed into N in the silica tube burner hearth
2Air-flow, the heating quartz transistor, insulation 2-6h, furnace cooling, be down to 100 ℃ when the temperature of silica tube burner hearth afterwards, closes N
2Air-flow, design parameter sees the following form:
The processing parameter of each sample of table 1
| Sample | Calcination temperature (℃) | Calcination time (h) | N 2Airshed (sccm) |
| （1） | 300 | 2 | 75 |
| （2） | 350 | 2 | 85 |
| （3） | 400 | 2 | 95 |
| （4） | 450 | 2 | 105 |
| （5） | 500 | 2 | 115 |
| （6） | 550 | 2 | 125 |
| （7） | 600 | 2 | 135 |
| （8） | 650 | 2 | 150 |
| （9） | 500 | 4 | 115 |
| （10） | 500 | 6 | 115 |
Fig. 1 is the powder x-ray diffraction spectrum of the sample (7) that obtains of the present embodiment, shows that the fluorescent powder product that obtains is carboritride fluorescent material, and it expresses general formula is g-C
3N
4, belong to the graphite laminate structure.
The emmission spectrum of the sample that the present embodiment obtains (1) ~ (8) as shown in Figure 2.Along with the rising of calcination temperature, the emission peak bandwidth is broadening gradually, and the emission band peak position is gradually to long wavelength's zone red shift.
The emmission spectrum of the sample that the present embodiment obtains (5), (9), (10) as shown in Figure 3.Under same calcination temperature, calcination time extends 6h from 2h, and the emission peak bandwidth is without considerable change, and the emission band peak position is slightly to long wavelength's zone red shift.
Fig. 4 is the excitation spectrum of the sample (7) that obtains of the present embodiment, and center excitation peak wavelength is 280nm, and excitation band has been contained the 240nm-400nm(UV-light) interval.The excitation spectrum of the excitation spectrum of the sample that the present embodiment obtains (1) ~ (6), (8) ~ (10) and sample (7) is similar, and also near 280nm, excitation band has been contained the 240nm-400nm(UV-light to center excitation peak wavelength equally) interval.
Fig. 5 is the fluorescent emission life-span collection of illustrative plates of the resulting sample of the present embodiment (1), (4), (8), as seen from the figure, resulting fluorescent material is nanosecond order in the fluorescence lifetime of 480nm emission peak, is conducive to gained carboritride fluorescent material in illumination and shows the application in field.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (4)
1. the preparation method of a carboritride fluorescent material, is characterized in that, comprises the following steps:
With trimeric cyanamide calcination under nitrogen atmosphere, calcination temperature is 300 ℃-650 ℃, and calcination time is 2-6h, obtains carboritride fluorescent material after furnace cooling.
2. the preparation method of carboritride fluorescent material according to claim 1, is characterized in that, and is described with trimeric cyanamide calcination under nitrogen atmosphere, is specially:
With the trimeric cyanamide alumina crucible of packing into, the silica tube burner hearth calcination of alumina crucible being put into atmosphere furnace stablely in the silica tube burner hearth in the calcination process passes into the N that flow is 75-150sccm
2Air-flow.
3. the preparation method of carboritride fluorescent material according to claim 2, is characterized in that, after the calcination end of processing, is down to 100 ℃ when the temperature of silica tube burner hearth, closes N
2Air-flow.
4. the carboritride fluorescent material that obtains of the preparation method of the described carboritride fluorescent material of claim 1 ~ 3, is characterized in that, it expresses general formula is g-C
3N
4, be the graphite laminate structure.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601162A (en) * | 2013-11-26 | 2014-02-26 | 天津大学 | Preparation method of graphite type carbon nitride nanotubes |
| CN105154075A (en) * | 2015-09-15 | 2015-12-16 | 郑州大学 | Preparation method of graphite-phase carbon nitride solid fluorescent powder and application thereof in light fingerprint extraction |
| CN106243388A (en) * | 2016-07-27 | 2016-12-21 | 华南理工大学 | A kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function and preparation method and application |
| CN106433616A (en) * | 2016-08-03 | 2017-02-22 | 江苏纳盾科技有限公司 | Ultraviolet fluorescence material and preparation method thereof |
| CN106479492A (en) * | 2016-09-14 | 2017-03-08 | 武汉理工大学 | A kind of polymolecularity g C3N4The preparation method of quantum dot |
| CN106744743A (en) * | 2016-12-05 | 2017-05-31 | 北京工业大学 | A kind of one-step synthesis water solubility g C3N4The preparation method of material |
| CN106833609A (en) * | 2017-01-19 | 2017-06-13 | 福州大学 | A kind of green fluorescence nitrogenizes the preparation method of carbon dust |
| CN111302315A (en) * | 2020-03-16 | 2020-06-19 | 昆明学院 | Preparation method and application of nitrogen-carbon-based light conversion agent, light conversion plastic film and preparation method thereof |
| CN116333733A (en) * | 2023-03-28 | 2023-06-27 | 安阳工学院 | Method for preparing high quantum efficiency ultraviolet emission melem fluorescent powder in ammonia atmosphere |
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| JP2008101094A (en) * | 2006-10-18 | 2008-05-01 | Shimane Pref Gov | Method for producing fluorescent material |
| CN102218339A (en) * | 2011-04-01 | 2011-10-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Graphite-phase carbon and nitrogen compound powder, as well as preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601162A (en) * | 2013-11-26 | 2014-02-26 | 天津大学 | Preparation method of graphite type carbon nitride nanotubes |
| CN105154075A (en) * | 2015-09-15 | 2015-12-16 | 郑州大学 | Preparation method of graphite-phase carbon nitride solid fluorescent powder and application thereof in light fingerprint extraction |
| CN106243388A (en) * | 2016-07-27 | 2016-12-21 | 华南理工大学 | A kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function and preparation method and application |
| CN106433616A (en) * | 2016-08-03 | 2017-02-22 | 江苏纳盾科技有限公司 | Ultraviolet fluorescence material and preparation method thereof |
| CN106433616B (en) * | 2016-08-03 | 2018-12-21 | 江苏纳盾科技有限公司 | A kind of ultraviolet fluorescent material and preparation method thereof |
| CN106479492A (en) * | 2016-09-14 | 2017-03-08 | 武汉理工大学 | A kind of polymolecularity g C3N4The preparation method of quantum dot |
| CN106744743A (en) * | 2016-12-05 | 2017-05-31 | 北京工业大学 | A kind of one-step synthesis water solubility g C3N4The preparation method of material |
| CN106833609A (en) * | 2017-01-19 | 2017-06-13 | 福州大学 | A kind of green fluorescence nitrogenizes the preparation method of carbon dust |
| CN111302315A (en) * | 2020-03-16 | 2020-06-19 | 昆明学院 | Preparation method and application of nitrogen-carbon-based light conversion agent, light conversion plastic film and preparation method thereof |
| CN111302315B (en) * | 2020-03-16 | 2023-02-17 | 昆明学院 | Preparation method and application of nitrogen-carbon-based light conversion agent, light conversion plastic film and preparation method thereof |
| CN116333733A (en) * | 2023-03-28 | 2023-06-27 | 安阳工学院 | Method for preparing high quantum efficiency ultraviolet emission melem fluorescent powder in ammonia atmosphere |
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Application publication date: 20130508 |