CN107502338A - A kind of amine-modified g C of phonetic Le3N4Blue colour fluorescent powder and its preparation and application - Google Patents
A kind of amine-modified g C of phonetic Le3N4Blue colour fluorescent powder and its preparation and application Download PDFInfo
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- CN107502338A CN107502338A CN201710749282.9A CN201710749282A CN107502338A CN 107502338 A CN107502338 A CN 107502338A CN 201710749282 A CN201710749282 A CN 201710749282A CN 107502338 A CN107502338 A CN 107502338A
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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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- 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
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
Abstract
The invention discloses a kind of amine-modified g C of phonetic Le3N4Blue colour fluorescent powder and its preparation and application.The composition of the fluorescent material is phonetic Le amine (C6N10H6) modification class graphite phase carbon nitride (g C3N4) compound, the synthesis of the fluorescent material is using melamine as raw material, reacts to obtain by pyrocondensation.The present invention has advantages below compared with prior art：Raw material rich reserves, fluorescent material is free of heavy metal, nontoxic, environmentally friendly, has good chemical stability and biocompatibility；The luminous efficiency of fluorescent material disclosed in this invention is than pure g C3N4Light-emitting phosphor efficiency improves more than three times；The present invention is not only prepared for a kind of blue colour fluorescent powder, and obtains a kind of suitable for making high quality g C3N4The predecessor of blue carbon nitrogen quantum dot, the quantum dot can be as the luminescent layers of flexible and transparent display device.
Description
Technical field
The invention belongs to powder metallurgical technology, more particularly to a kind of inorganic non-metallic blueness of not metal ion are glimmering
Light powder and its technology of preparing, it is specially phonetic to strangle amine-modified g-C3N4Nonmetallic blue colour fluorescent powder material composition, preparation method and
Using.
Background technology
Blue light be form visible ray important spectral component, using blue light by lower conversion can be further converted into it is red,
Orange, yellow, green other color visibles.But in illumination and field of information display, the control and synthesis of blue colour fluorescent powder and blue light
The exploitation of device is particularly difficult.The blue colour fluorescent powder used in the past mainly has, such as aluminate BaMgAl10O17：Eu2+(BAM), silicon
Hydrochlorate M3MgSi2O8：Eu2+(M=Ba, Sr), Y2SiO5：Ce3+And sulfide ZnS：Cu, Ag etc., this kind of fluorescent material are usually used
Rare earth or transition-metal ion are as activator, and not only synthesis temperature is high, technique is harsh, and price is high.Further, since
Blue photons energy is high, and in use with the accumulation of environment temperature and time effect, the centre of luminescence or defect center are at any time
Between extend and slowly change (such as Eu2+It is oxidized to Eu3+), cause luminous intensity gradually to reduce.
There is tranmitting frequency to change with change in size, launch line width for quantum dot (Quantum Dot) luminescent material, hair
The of a relatively high and higher photostability of photo-quantum efficiency and the characteristic of solution processing, it is that following illumination develops with Display Technique
One of scheme.Between Past 30 Years, inorganic-quantum-dot luminescent material has been attempted to be ground applied to photoelectronics and biomedicine etc.
Study carefully field, and the quantum dot reported at present mainly has II-VI group CdSe (S/Te), iii-v InP (As, Sb) and your gold
Belong to Ag2Se (S, Te) etc., but this kind of quantum dot contains heavy metal element, and use environment produces pollution, does not meet green want
Ask.2013, Xie Yi seminars of China Science ＆ Technology University reported a kind of C with graphene two-dimensional slice structure3N4(g-
C3N4) quantum dot light emitting material (J.Am.Chem.Soc, 2013,135,18-21).C3N4Quantum dot is free of heavy metal, not only without
Poison is harmless, and stable with chemical property with good biocompatibility.But g-C3N4Blue luminescence efficiency is than relatively low, and one
The blue fluorescent material that can not be directly activated with rare earth with transition-metal ion compares favourably.Current all documents all think that carbon nitrogenizes
The blue-light-emitting of thing derives from the g-C of graphite-phase layer structure3N4, but we are by showing luminescence mechanism research, g-C3N4Hair
Light efficiency is strongly depend on surface group.By controlling synthesis technique, in g-C3N4Surface forms the amine-modified g-C of phonetic Le3N4It is multiple
Structure is closed, light-emitting phosphor intensity can be made to improve more than three times.
Thus, the present invention develops a kind of amine-modified g-C of phonetic Le by improving synthesis technique3N4Blue colour fluorescent powder.Should
Blue colour fluorescent powder is neither graphite-phase C3N4, nor phonetic Le amine or triazine structure, but the graphite-phase C that phonetic Le is amine-modified3N4It is multiple
Compound.The present invention is not only prepared for a kind of blue colour fluorescent powder, and obtains a kind of suitable for making high quality g-C3N4Blue carbon nitrogen
The predecessor of quantum dot.By the use of the fluorescent material as presoma, the g-C prepared is peeled off by ultrasound3N4Quantum dot light emitting efficiency is widely different
It is so very high.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of amine-modified g-C of phonetic Le3N4Blueness is glimmering
Light powder.
The present invention is achieved by the following technical solutions：A kind of amine-modified g-C of phonetic Le3N4The preparation of blue colour fluorescent powder
Method, it is characterised in that comprise the following steps：Take melamine to calcine 1~3h at 450~650 DEG C, cool to room temperature with the furnace
Crushing grinding is taken out afterwards obtains inorganic non-metallic blue colour fluorescent powder.
As further improvement of these options, the calcination process is carried out in sintering furnace.
As further improvement of these options, the calcination process is carried out in air or nitrogen atmosphere.
As further improvement of these options, the temperature calcined in air atmosphere is 450 DEG C, and calcination time is
2h。
As further improvement of these options, the temperature calcined in nitrogen atmosphere is 500 DEG C, and calcination time is
2h。
The present invention also provides a kind of phonetic Le prepared by the above method amine-modified g-C3N4Blue colour fluorescent powder.
In addition the present invention also provides a kind of g-C amine-modified using above-mentioned phonetic Le3N4Blue colour fluorescent powder is prepared as quantum dot
Presoma, it is characterised in that：The amine-modified g-C of the phonetic Le3N4Blue quantum dot, is prepared by the following, and will weigh
Profit requires the amine-modified g-C of the phonetic Le described in 53N4Blue colour fluorescent powder carries out ultrasonic stripping in polar solvent, by institute after stripping
Obtain solution and carry out centrifugal treating, supernatant liquor is taken after removing precipitation, obtain the amine-modified g-C of the phonetic Le3N4Quantum dot.
As further improvement of these options, the polar solvent is water or ethanol.
Meanwhile the present invention also provides 0LED or flexible and transparent display device that above-mentioned blue light-emitting layer is applied.
The present invention has advantages below compared with prior art：Novel blue fluorescent material disclosed by the invention, it is not relevant
Class graphite phase carbon nitride (g-C described in document3N4), but phonetic Le amine (C6N10H6) modification class graphite phase carbon nitride (g-
C3N4) compound；The fluorescent material, it is a kind of inorganic non-metallic material without rare earth and transition-metal ion activator, its
The carbon contained and nitrogen rich reserves in the earth；The material luminous efficiency is high, and external quantum efficiency reaches more than 22%, is to adopt
Class graphite phase carbon nitride (the g-C prepared with common process3N4) three times of blue colour fluorescent powder luminous intensity；Closed using the present invention
Au bleu fluorescent material as presoma, by water or ethanol polar solvent ultrasound peel off and prepare quantum dot, it is and existing
II-VI group CdSe (S/Te), iii-v InP (As, Sb) and precious metals ag2Se (S, Te) etc. is compared, and the present invention does what is prepared
Quantum dot has good chemical stability and biocompatibility, nontoxic, environmentally friendly and cheap；Using upper
Quantum dot is stated as blue light-emitting layer.In addition the present invention demonstrates its possibility applied in OLED first.
Brief description of the drawings
In Fig. 1 embodiments 1 under air atmosphere different temperatures synthetic powder x-ray diffraction pattern.
In Fig. 2 embodiments 1 under air atmosphere different temperatures synthetic powder emission spectrum.
In Fig. 3 embodiments 1 under air atmosphere different temperatures synthetic powder excitation spectrum.
In Fig. 4 embodiments 2 under nitrogen atmosphere different temperatures synthetic powder x-ray diffraction pattern.
In Fig. 5 embodiments 2 under nitrogen atmosphere different temperatures synthetic powder emission spectrum.
In Fig. 6 embodiments 2 under nitrogen atmosphere different temperatures synthetic powder excitation spectrum.
Nitrogen atmosphere encloses synthetic powder emission spectrum under the differential responses time in Fig. 7 embodiments 3.
It is phonetic in Fig. 8 embodiments 4 to strangle amine-modified g-C3N4The TEM figures of quantum dot.
Fig. 9 is OLED basic structure schematic diagram.
The emission spectrum of OLED and the luminosity curve under different voltages in Figure 10 embodiments 5.
Working example figure of the OLED under 21V voltages in Figure 11 embodiments 5.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
The invention provides a kind of nonmetallic blue colour fluorescent powder.Specifically, the nonmetallic blue colour fluorescent powder is phonetic Le amine
(C6N10H6) modification class graphite phase carbon nitride (g-C3N4) compound, in Two-phase composite structure, the phonetic quality strangled shared by amine phase
Fraction is 0 ＜ x ＜ 100%.Its launch wavelength is 450nm or so, is typical blue colour fluorescent powder.Synthesized reaction production of the invention
Thing, act not only as blue colour fluorescent powder exclusive use, and the predecessor that can be prepared as nano material.By in polarity
Reaction product ultrasound is peeled off in solvent, and then blue nano particle can be prepared.The nano particle prepared using the predecessor,
Can be as OLED (Organic Light Emitting Diode) and the blue light-emitting layer of flexible and transparent display device.
Embodiment 1
Weigh appropriate melamine, load corundum crucible, be put into van-type stove, respectively at 450,500 under atmospheric environment,
550,600,650 DEG C are reacted 2 hours, and reaction cools to room temperature with the furnace after terminating.After sample takes out from stove, through crushing and grinding
After processing, structure and performance test are carried out.
As shown in figure 1, by the XRD spectrum analysis shows to synthesizing fluorescent material under different temperatures, melamine is big
Product under compression ring border in 450 DEG C of high temperature polymerizations is mainly phonetic Le amine and g-C3N4Phase, in addition containing a small amount of still unreacted trimerization
Cyanamide.As reaction temperature raises, the melamine diffraction maximum of residual disappears, and phonetic Le amine phase diffracted intensity gradually weakens, g-C3N4
Phase diffraction maximum gradually strengthens, and illustrates g-C3N4The temperature that accompanies rise crystallinity gradually improves.
Fig. 2 is emission spectrum of the synthesized fluorescent material in the case where 365nm is excited at different temperatures.From Fig. 2 it is known that
The emission spectrum scope of fluorescent material is 400-580nm.The luminous most strong of fluorescent material, Emission Spectrum Peals are synthesized at 450 DEG C
It is ideal blue light for 451nm.650 DEG C are increased to from 450 with temperature, luminous intensity gradually reduces and emission spectrum peak
It is worth gradual red shift.
Fig. 3 is the excitation spectrum that monitoring 470nm transmittings measure.It can also be learnt from Fig. 3, fluorescent material is synthesized at 450 DEG C
Excite it is most strong.Raised with temperature, not only excitation intensity reduces, and excitation spectrum configuration changes.Excitation spectrum configuration
Change, mainly due to caused by the change of electron excitation level structure.
Embodiment 2
Weigh appropriate melamine, load corundum crucible, be put into quartz tube furnace, under nitrogen protection respectively at 450,
500,550,600,650 DEG C are reacted 2 hours, and reaction cools to room temperature with the furnace after terminating.After sample takes out from stove, through crush with
After milled processed, structure and performance test are carried out.
As shown in figure 4, in a nitrogen atmosphere in the XRD spectrum variation with temperature of synthetic sample and Fig. 2 under atmospheric environment
Synthetic sample variation with temperature is similar.But phonetic Le amine diffraction maximum in 450 and 500 DEG C of synthetic sample XRD spectrums is contrasted respectively
Relative altitude is it can be found that the phonetic Le amine content under identical temperature conditionss in a nitrogen atmosphere in synthetic sample is relatively more.Knot
From the point of view of closing Fig. 5 emission spectrum, the phonetic relative amount for strangling amine is not The more the better, 500 DEG C of conjunctions in a nitrogen atmosphere in fluorescent material
It is most strong into light-emitting phosphor；And 450 DEG C of synthetizing phosphor powders are luminous most strong in air atmosphere.Fig. 5 and Fig. 6 is respectively in nitrogen gas
The transmitting of different temperatures synthetizing phosphor powder and excitation spectrum under atmosphere.From the point of view of excitation spectrum, the dominant mechanism of blue-light-emitting is produced
Be lone pair electrons (LP) do not occupied to high energy state π * antibonding orbitals transition (LP- π *) and π bonding orbitals to π * antibonding orbitals
Caused by transition (π-π *).Comparison diagram 4 and Fig. 6, in a nitrogen atmosphere π-π * the excitation intensities of synthetizing phosphor powder be significantly higher than big
The excitation intensity of synthetizing phosphor powder under compression ring border, the fluorescent material that this explanation synthesizes in a nitrogen atmosphere are advantageously hexa-atomic in C-N
The formation of ring and pi bond.Show with reference to XRD and spectrofluorimetry, the phonetic presence for strangling amine is to improve the necessary bar of luminescent properties
Part.This is probably because phonetic Le amine is present, and on the one hand protects g-C3N4The non-bonding lone pair electrons in surface, it is on the other hand good to be formed
Good triazine ring structure and pi bond provides necessary condition, because g-C3N4Formation to have melamine condensation first be phonetic Le amine
(or how phonetic Le amine triazine ring structure), then g-C is polymerized to by phonetic Le amine3N4。
Embodiment 3
Fluorescent material synthetic method is same as Example 2, and reaction temperature is 500 DEG C, and the reaction time asks 1,2,3 hour respectively.
Synthesized phosphor emission spectrum is as shown in Figure 7.Fig. 2,5,7 show that synthesis blue colour fluorescent powder optimum condition is in nitrogen atmosphere
Lower 500 DEG C polymerize 2 hours.
Embodiment 4
It is phonetic to strangle amine-modified g-C3N4The preparation of quantum dot, using the fluorescent material of above-mentioned synthesis, disperse in deionized water, profit
Ultrasonic stripping is carried out with ultrasonic generator, resulting solution is subjected to centrifugal treating after stripping, bulky grain precipitation is removed, obtains nanometer
Particle supernatant liquor, it is made phonetic and strangles amine-modified g-C3N4Quantum dot.Quantum dot is zero dimension material, and it is scattered in a solvent, then
Utilize the direct spin coating of solution.TEM test results are as shown in figure 8, prepared spherical quantum dots particle.
Embodiment 5
The amine-modified g-C of phonetic Le obtained with embodiment 43N4Quantum dot as blue light-emitting layer, the OLED being prepared into or
Person's flexible and transparent display device.
The basic structure for the OLED that Fig. 9 shows, on ITO conducting glass substrates, spin coating hole injection layer PEDOT successively：
PSS, wait drying after again spin coating hole transmission layer PVK, again dry after spin coating luminescent layer blueness nano particle, be finally deposited successively
TPBi, LiF and Al obtain OLED.
The emission spectrum of the device and luminosity under different voltages are as shown in Figure 10, the emission spectrum of device with
The emission spectrum peak of nano particle is consistent, so device just derives from blue nano particle.Device is when voltage is 21V
Illuminated diagram it is as shown in figure 11, OLED emits a brilliant light, its blue quantum dot can be used for prepare LED component.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
- A kind of 1. amine-modified g-C of phonetic Le3N4The preparation method of blue colour fluorescent powder, it is characterised in that comprise the following steps：Take trimerization Cyanamide calcines 1~3h at 450~650 DEG C, and taking-up crushing grinding obtains the blue colour fluorescent powder after cooling to room temperature with the furnace.
- A kind of 2. amine-modified g-C of phonetic Le as claimed in claim 13N4The preparation method of blue colour fluorescent powder, it is characterised in that：Institute Calcination process is stated to carry out in sintering furnace.
- A kind of 3. amine-modified g-C of phonetic Le as claimed in claim 13N4The preparation method of blue colour fluorescent powder, it is characterised in that：Institute Calcination process is stated to carry out in air or nitrogen atmosphere.
- A kind of 4. amine-modified g-C of phonetic Le as claimed in claim 33N4The preparation method of blue colour fluorescent powder, it is characterised in that： The temperature calcined in air atmosphere is 450 DEG C, calcination time 2h.
- A kind of 5. amine-modified g-C of phonetic Le as claimed in claim 33N4The preparation method of blue colour fluorescent powder, it is characterised in that： The temperature calcined in nitrogen atmosphere is 500 DEG C, calcination time 2h.
- A kind of 6. amine-modified g-C of phonetic Le3N4Blue colour fluorescent powder, it is characterised in that the phonetic Le is amine-modifiedg-C3N4Blue colour fluorescent powder is prepared by any method in such as claim 1 to 5.
- 7. a kind of strangle amine-modified g-C using phonetic3N4Blue light-emitting layer of the quantum dot as display device, it is characterised in that：It is described In blue light-emitting layer amine-modified g-C is strangled using phonetic3N4Quantum dot, the quantum dot are prepared by the following, will by right Seek the amine-modified g-C of the phonetic Le described in 63N4Blue colour fluorescent powder carries out ultrasonic stripping in polar solvent, after stripping that gained is molten Liquid carries out centrifugal treating, and supernatant liquor is taken after removing lower sediment, obtains the amine-modified g-C of the phonetic Le3N4Quantum dot.
- 8. a kind of as claimed in claim 7 strangle amine-modified g-C using phonetic3N4Quantum dot blue light-emitting layer, it is characterised in that：Institute It is water or ethanol to state polar solvent.
- A kind of 9. OLED using blue light-emitting layer as claimed in claim 7 or 8.
- A kind of 10. flexible and transparent display device using blue light-emitting layer as claimed in claim 7 or 8.
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Cited By (5)
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| CN108276995A (en) * | 2018-01-23 | 2018-07-13 | 广东工业大学 | Application of the melem carbon-nitrogen material as long after glow luminous material |
| CN109294571A (en) * | 2018-12-12 | 2019-02-01 | 临沂大学 | A kind of carbon nitrogen powder yellow fluorescent material and preparation method |
| CN112420972A (en) * | 2020-11-26 | 2021-02-26 | 西安航天三沃化学有限公司 | Graphite-phase carbon nitride quantum dot film and preparation method and application thereof |
| 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 |
| 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276995A (en) * | 2018-01-23 | 2018-07-13 | 广东工业大学 | Application of the melem carbon-nitrogen material as long after glow luminous material |
| CN109294571A (en) * | 2018-12-12 | 2019-02-01 | 临沂大学 | A kind of carbon nitrogen powder yellow fluorescent material and preparation method |
| CN109294571B (en) * | 2018-12-12 | 2021-04-30 | 临沂大学 | Carbon-nitrogen powder yellow fluorescent material and preparation method thereof |
| CN112420972A (en) * | 2020-11-26 | 2021-02-26 | 西安航天三沃化学有限公司 | Graphite-phase carbon nitride quantum dot film and preparation method and application thereof |
| 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 |
| 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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