CN102827599B - Preparation method of red-green-blue blended white light phosphor - Google Patents
Preparation method of red-green-blue blended white light phosphor Download PDFInfo
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- CN102827599B CN102827599B CN2012102952081A CN201210295208A CN102827599B CN 102827599 B CN102827599 B CN 102827599B CN 2012102952081 A CN2012102952081 A CN 2012102952081A CN 201210295208 A CN201210295208 A CN 201210295208A CN 102827599 B CN102827599 B CN 102827599B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract 5
- KQHXBDOEECKORE-UHFFFAOYSA-L beryllium sulfate Chemical compound [Be+2].[O-]S([O-])(=O)=O KQHXBDOEECKORE-UHFFFAOYSA-L 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- NNMXSTWQJRPBJZ-UHFFFAOYSA-K europium(iii) chloride Chemical compound Cl[Eu](Cl)Cl NNMXSTWQJRPBJZ-UHFFFAOYSA-K 0.000 claims abstract description 12
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 81
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 75
- 239000000843 powder Substances 0.000 claims description 74
- 238000003756 stirring Methods 0.000 claims description 68
- 238000000967 suction filtration Methods 0.000 claims description 66
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 60
- 239000012065 filter cake Substances 0.000 claims description 56
- 238000006243 chemical reaction Methods 0.000 claims description 54
- 238000009835 boiling Methods 0.000 claims description 53
- 239000000047 product Substances 0.000 claims description 53
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 44
- 229960005419 nitrogen Drugs 0.000 claims description 39
- 239000000126 substance Substances 0.000 claims description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 30
- 238000001291 vacuum drying Methods 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical class CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000001914 filtration Methods 0.000 claims description 22
- RWZYAGGXGHYGMB-UHFFFAOYSA-N anthranilic acid Chemical compound NC1=CC=CC=C1C(O)=O RWZYAGGXGHYGMB-UHFFFAOYSA-N 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 18
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 16
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 claims description 15
- KHAVLLBUVKBTBG-UHFFFAOYSA-N caproleic acid Natural products OC(=O)CCCCCCCC=C KHAVLLBUVKBTBG-UHFFFAOYSA-N 0.000 claims description 15
- 229960002703 undecylenic acid Drugs 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 9
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 9
- TXBBUSUXYMIVOS-UHFFFAOYSA-N thenoyltrifluoroacetone Chemical compound FC(F)(F)C(=O)CC(=O)C1=CC=CS1 TXBBUSUXYMIVOS-UHFFFAOYSA-N 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 8
- MVVGSPCXHRFDDR-UHFFFAOYSA-N 2-(1,3-benzothiazol-2-yl)phenol Chemical compound OC1=CC=CC=C1C1=NC2=CC=CC=C2S1 MVVGSPCXHRFDDR-UHFFFAOYSA-N 0.000 claims description 7
- 238000006424 Flood reaction Methods 0.000 claims description 6
- KIDXYAWWICJAFK-UHFFFAOYSA-N O.[Na].OC Chemical compound O.[Na].OC KIDXYAWWICJAFK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 229910052790 beryllium Inorganic materials 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 5
- 229960001701 chloroform Drugs 0.000 claims description 5
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 4
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- MWKMXMBITFXXBI-UHFFFAOYSA-N CO.OC1=C(C=CC=C1)C=1SC2=C(N1)C=CC=C2 Chemical compound CO.OC1=C(C=CC=C1)C=1SC2=C(N1)C=CC=C2 MWKMXMBITFXXBI-UHFFFAOYSA-N 0.000 claims description 2
- BWFOVCJXJSLXDR-UHFFFAOYSA-N CO.S1C=NC2=C1C=CC=C2 Chemical compound CO.S1C=NC2=C1C=CC=C2 BWFOVCJXJSLXDR-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 241001062009 Indigofera Species 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims description 2
- 229910000474 mercury oxide Inorganic materials 0.000 claims description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229940083608 sodium hydroxide Drugs 0.000 claims description 2
- 238000004611 spectroscopical analysis Methods 0.000 claims description 2
- 230000002459 sustained effect Effects 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 abstract description 7
- 230000000171 quenching effect Effects 0.000 abstract description 4
- 238000010791 quenching Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- -1 rare earth small molecules Chemical class 0.000 description 2
- VBTRLUDEPKOOPO-UHFFFAOYSA-K 2-aminobenzoic acid europium(3+) trichloride Chemical compound C(C=1C(N)=CC=CC1)(=O)O.[Eu+3].[Cl-].[Cl-].[Cl-] VBTRLUDEPKOOPO-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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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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- Luminescent Compositions (AREA)
Abstract
The invention relates to a preparation method of red-green-blue blended white light phosphor, which adopts europium chloride, terbium chloride, and beryllium sulfate as raw materials, and comprises the following steps: firstly preparing red, green, and blue rare earth complexes, then preparing red, green, and blue monochromatic polymers, finally blending the red, green, and blue monochromatic polymers in proportion to synthesize the white light phosphor; the preparation method is advanced in process, detailed and accurate in data; the white light phosphor has high luminous efficiency, and good luminous purity, has color coordinates of x=0.3253 and y=0.3301, and emits white light; the preparation method can effectively prevent the quenching phenomenon during doping, and is an ideal method for preparing white light rare earth phosphor.
Description
Technical field
The present invention relates to a kind of preparation method of RGB blend white emitting fluorescent powder, belong to the technical field of luminescent material preparation and application.
Background technology
The white light LEDs photodiode has advantages of that physical dimension is little, energy consumption is low, the life-span is long, be called as the 4th generation green light source, in industrial circle and the product for civilian use, obtained application.White emitting fluorescent powder synthetic mainly contains two kinds of approach, the one, rare earth small molecules complex compound directly is doped in polymer matrix and obtains doping type white light high polymer fluorescent material, this method technique is simple, but exist be separated, the problem of quenching of fluorescence and bad dispersibility; Another kind is first to synthesize the rare earth complex monomer with reactive behavior, then with other organic monomer polymerizations, obtains the bonding type high-molecular copolymer, or on rare earth ion and macromolecular chain, ligand groups such as carboxyl, sulfonic group react, and obtain the rare earth high polymer title complex; Facts have proved that the fluorescence intensity of monochromatic polymkeric substance is greater than the fluorescence intensity of three primary colours doping type polymkeric substance.
Summary of the invention
Goal of the invention
The objective of the invention is the situation for background technology, first prepare the monochromatic polymkeric substance of red, green, blue, then by the monochromatic polymer blending of red, green, blue, obtain white emitting fluorescent powder, concentration quenching effect while reducing monochromatic title complex and polymer matrix doping, to increase substantially the luminous intensity of white emitting fluorescent powder.
Technical scheme
The chemical substance material used is: Europium trichloride, α-thenoyltrifluoroacetone, 10 hendecenoic acid, terbium chloride, anthranilic acid, beryllium sulfate, 2-(2-hydroxy phenyl) benzothiazole, α-methacrylic acid, methyl methacrylate, Diisopropyl azodicarboxylate, sodium hydroxide, trichloromethane, dehydrated alcohol, anhydrous methanol, dimethyl sulfoxide (DMSO), nitrogen, it is as follows that it prepares consumption: with gram, milliliter, centimetre
3For measure unit
Europium trichloride: EuCl
36H
2O 0.3663g ± 0.0001g
α-thenoyltrifluoroacetone: C
8H
5F
3O
2S 0.6664g ± 0.0001g
10 hendecenoic acid: C
11H
20O
21.5mL ± 0.01mL
Terbium chloride: TbCl
36H
2O 0.3733g ± 0.0001g
Anthranilic acid: C
7H
7NO
20.4114g ± 0.0001g
Beryllium sulfate: BeSO
44H
2O 0.3542g ± 0.0001g
2-(2-hydroxy phenyl) benzothiazole: C
13H
9NOS 0.4544g ± 0.0001g
α-methacrylic acid: C
4H
6O
21.0mL ± 0.01mL
Methyl methacrylate: C
5H
8O
25.0mL ± 0.1mL
Diisopropyl azodicarboxylate: C
8H
12N
40.0300g ± 0.0001g
Sodium hydroxide: NaOH 20g ± 0.1g
Trichloromethane: CHCl
3500mL ± 10mL
Dehydrated alcohol: C
2H
6O 5000mL ± 10mL
Anhydrous methanol: CH
4O 2000mL ± 10mL
Dimethyl sulfoxide (DMSO): C
2H
6OS 1500mL ± 1mL
Nitrogen: N
210000cm
3± 100cm
3
The preparation method is as follows:
(1) obtain solution
Take Europium trichloride 0.3663g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the Europium trichloride ethanolic soln of 0.2mol/L;
Take α-thenoyltrifluoroacetone 0.6664g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, the α of one-tenth 0.6mol/L-thenoyltrifluoroacetone ethanolic soln;
Take 10 hendecenoic acid 1.218mL ± 0.001mL, measure dehydrated alcohol 30.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the 10 hendecenoic acid ethanolic soln of 0.2mol/L;
Weighing sodium hydroxide 20.0g ± 0.1g, measure dehydrated alcohol 50.0mL+ ± 0.1mL, is placed in beaker, stirs 5min with agitator, becomes the sodium hydroxide ethanolic soln of 1mol/L;
Take terbium chloride 0.3733g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the terbium chloride ethanolic soln of 0.2mol/L;
Take anthranilic acid 0.4114g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the Europium trichloride anthranilic acid ethanolic soln of 0.6mol/L;
Take beryllium sulfate 0.3542g ± 0.0001g, measure anhydrous methanol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the beryllium sulfate methanol solution of 0.4mol/L;
Take 2-(2-hydroxy phenyl) benzothiazole 0.4544g ± 0.0001g, measure anhydrous methanol 8.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become 2-(2-hydroxy phenyl) the benzothiazole methanol solution of 0.25mol/L;
Weighing sodium hydroxide 20.0g ± 0.1g, measure anhydrous methanol 50.0mL+ ± 0.1mL, is placed in beaker, stirs 5min with agitator, becomes the sodium hydrate methanol solution of 1mol/L;
(2) prepare red light fluorescent powder
Prepare red light fluorescent powder and carry out in there-necked flask, complete in heating, stirring, dropping solution process;
α-thenoyltrifluoroacetone ethanolic soln 5mL is added in dropping funnel, drip, rate of addition 1mL/min, stir on dropping limit, limit, and regulating the pH value is 6.5-7.0;
(3) prepare green light fluorescent powder
Prepare green light fluorescent powder and carry out in there-necked flask, complete in heating, stirring, dropping solution process;
10 hendecenoic acid ethanolic soln 5mL is added in there-necked flask, and opening electric heater, be heated to 50 ℃ ± 2 ℃, and turn on agitator stirs;
Terbium chloride ethanolic soln 5mL is added in dropping funnel, drip, rate of addition 1mL/min, stir on dropping limit, limit, time 5min;
Washing, suction filtration, be placed in beaker by the product filter cake, adds dehydrated alcohol 100mL, agitator treating 5min; Then carry out suction filtration; Washing, suction filtration repeat 5 times, obtain the product filter cake;
(4) prepare blue light fluorescent powder
Prepare blue light fluorescent powder and carry out in there-necked flask, complete in heating, stirring, dropping solution process;
By the 2-(2-hydroxy phenyl) benzothiazole methanol solution 5mL adds in there-necked flask; Opening electric heater, be heated to 50 ℃ ± 2 ℃; Turn on agitator stirs;
Stopped heating, stop stirring, and makes it with bottle is standing, be cooled to 25 ℃, and precipitation, obtains reaction soln;
(5) prepare the monochromatic polymkeric substance of the Eu glowed
The monochromatic polymkeric substance of the Eu that preparation glows carries out in four-hole boiling flask, complete under heating, water-bath, stirring, nitrogen protection;
Add initiator Diisopropyl azodicarboxylate 0.0074g ± 0.0001g;
Add solvent dimethyl sulfoxide (DMSO) 5.0mL ± 0.1mL;
Then four-hole boiling flask is carried out on the ultrasonic vibration instrument to ultrasonic vibration 30min, make its dissolving, become reaction soln;
Four-hole boiling flask and reaction soln are placed on cleansing bath tub, and water-bath water floods 4/5 of four-hole boiling flask volume, on four-hole boiling flask, inserts successively from left to right dropping funnel, agitator, pH meter, nitrogen tube;
(6) prepare the monochromatic polymkeric substance of Tb of green light
The monochromatic polymkeric substance of the Tb of preparation green light carries out in four-hole boiling flask, complete under heating, water-bath, stirring, nitrogen protection;
Add initiator Diisopropyl azodicarboxylate 0.0074g ± 0.0001g;
Add solvent dimethyl sulfoxide (DMSO) 5.0mL ± 0.1mL;
Then four-hole boiling flask is carried out on the ultrasonic vibration instrument to ultrasonic vibration 30min, make its dissolving, become reaction soln;
Four-hole boiling flask and reaction soln are placed on cleansing bath tub, and water-bath water floods 4/5 of four-hole boiling flask;
(7) prepare the monochromatic polymkeric substance of Be of blue light-emitting
The monochromatic polymkeric substance of Be for preparing blue light-emitting carries out in four-hole boiling flask, complete under heating, water-bath, stirring, nitrogen protection;
Add initiator Diisopropyl azodicarboxylate 0.0074g ± 0.0001g;
Add solvent dimethyl sulfoxide (DMSO) 5.0mL ± 0.1mL;
Then four-hole boiling flask is carried out on the ultrasonic vibration instrument to ultrasonic vibration 30min, make its dissolving, become reaction soln;
(8) blend prepares white emitting fluorescent powder
Prepare white emitting fluorescent powder and be the monochromatic polymkeric substance of Eu, the monochromatic polymkeric substance of Tb, Be monochrome polymer-doped, through mixing, dissolving, precipitation, filtration, drying, obtain white emitting fluorescent powder;
Take the monochromatic polymkeric substance 0.0100g ± 0.0001g of ruddiness Eu;
Take the monochromatic polymkeric substance 0.0138g ± 0.0001g of green glow Tb;
Take the monochromatic polymkeric substance 0.0046g ± 0.0001g of blue light Be;
Be placed in beaker, then add trichloromethane 10.0mL ± 0.1mL;
(10) detect, analyze, characterize
Pattern, color and luster, composition, the chemical physics performance of white emitting fluorescent powder to preparation detects, analyzes, characterizes;
By fluorescence spectrophotometer, carry out fluorescent spectroscopy;
Conclusion: white emitting fluorescent powder is solid-state white powder, and particle diameter≤2000nm, chromaticity coordinates are x=0.3253, and y=0.3301, emit white light;
(11) product stores
White emitting fluorescent powder to preparation is stored in brown transparent Glass Containers, and airtight keeping in Dark Place wants waterproof, protection against the tide, anti-acid-alkali salt to corrode, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has obvious advance, first prepares the red, green, blue rare earth compounding, then prepares the monochromatic polymkeric substance of red, green, blue, finally by the blend in proportion of the monochromatic polymkeric substance of red, green, blue, obtain white emitting fluorescent powder, this preparation method's technique advanced person, informative data is accurate, the white emitting fluorescent powder luminous efficiency is high, luminance purity is good, chromaticity coordinates x=0.3253, y=0.3301, Quenching in the time of can effectively preventing from adulterating is the desirable method for preparing white emitting fluorescent powder.
The accompanying drawing explanation
Fig. 1 is for preparing the state graph of red, green, blue title complex
Fig. 2 is for preparing the monochromatic state of polymer figure of red, green, blue
Fig. 3 is white emitting fluorescent powder polymer fluorescent spectrogram
Fig. 4 is white fluorescence powder polymer chromaticity coordinates figure
Shown in figure, list of numerals is as follows:
1, the first electric controller, 2, electric mantle, 3, there-necked flask, 4, the first dropping funnel, 5, the first control valve, 6, the first agitator, 7, the first pH meter, 8, reaction soln, 9, the first display screen, 10, the first pilot lamp, 11, first stirs modulator, 12, the first Heating temperature modulator, 13, the second electric controller, 14, cleansing bath tub, 15, four-hole boiling flask, 16, the second dropping funnel, 17, the second control valve, 18, the second agitator, 19, the second pH meter, 20, nitrogen tube, 21, nitrogen valve, 22, nitrogengas cylinder, 23, reaction soln, 24, second display screen, 25, the second pilot lamp, 26, second stirs modulator, 27, the second Heating temperature modulator, 28, nitrogen.
Embodiment
The invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, for preparing the state graph of red, green, blue rare earth compounding, it is correct that want each position, according to quantity proportioning, operation according to the order of sequence.
The value of the chemical substance that preparation is used, be to determine by the scope set in advance, with gram, milliliter, centimetre
3For measure unit.
The preparation of red, green, blue rare earth compounding, carry out respectively in there-necked flask, be to complete in the process of heating, stirring, adjusting potential of hydrogen;
The top of the first electric controller 1 is electric mantle 2, on electric mantle 2, puts there-necked flask 3, the first dropping funnel 4 and first is set from left to right controls net 5, the first agitator 6, the first pH meter 7 on there-necked flask 3; The first display screen 9, the first pilot lamp 10, the first stirring modulator 11, the first Heating temperature modulator 12 are set on the front panel of the first electric controller 1.
Shown in Figure 2, for preparing the monochromatic state of polymer figure of red, green, blue, it is correct that want each position, according to quantity proportioning, operation according to the order of sequence.
The preparation of the monochromatic polymkeric substance of red, green, blue, carry out respectively in four-hole boiling flask, complete under heating, stirring, water-bath, nitrogen protection;
The top of the second electric controller 13 is cleansing bath tub 14, on cleansing bath tub 14, puts four-hole boiling flask 15, on four-hole boiling flask 15 tops by left-to-right the second dropping funnel 16 and the second control valve 17, the second agitator 18, the second pH meter 19, the nitrogen tube 20 of arranging; Nitrogen tube 20 connects nitrogen valve 21, nitrogengas cylinder 22; Second display screen 24, the second pilot lamp 25, the second stirring modulator 26, the second Heating temperature modulator 27 are set on the front panel of the second electric controller 13; In four-hole boiling flask 15, be reaction soln 23, nitrogen 28.
Shown in Figure 3, be white emitting fluorescent powder polymer fluorescent spectrogram, as can be known in figure: the emission peak that wherein is positioned at the 430nm place belongs to the emission of the monochromatic polymkeric substance of Be; 488 and the emission peak at 543nm place belong to the characteristic emission of Tb (III) ion in the monochromatic polymkeric substance of Tb, corresponding to
5D
4-
7F
6,
5D
4-
7F
5Transition; 590, the emission peak of 611 and 650 nm belongs to the characteristic emission of Eu (III) ion in the monochromatic polymkeric substance of Eu, corresponding to
5D
0-
7F
1,
5D
0-
7F
2,
5D
0-
7F
3Transition.
Shown in Figure 4, be white fluorescence powder polymer chromaticity coordinates figure, chromaticity coordinates x=0.3253 as can be known in figure, y=0.3301, emit white light.
Claims (3)
1. the preparation method of a RGB blend white emitting fluorescent powder, it is characterized in that: the chemical substance material of use is: Europium trichloride, α-thenoyltrifluoroacetone, 10 hendecenoic acid, terbium chloride, anthranilic acid, beryllium sulfate, 2-(2-hydroxy phenyl) benzothiazole, α-methacrylic acid, methyl methacrylate, Diisopropyl azodicarboxylate, sodium hydroxide, trichloromethane, dehydrated alcohol, anhydrous methanol, dimethyl sulfoxide (DMSO), nitrogen, it is as follows that it prepares consumption: with gram, milliliter, centimetre
3For measure unit
The preparation method is as follows:
(1) obtain solution
1. prepare the Europium trichloride ethanolic soln
Take Europium trichloride 0.3663g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the Europium trichloride ethanolic soln of 0.2mol/L;
2. prepare α-thenoyltrifluoroacetone ethanolic soln
Take α-thenoyltrifluoroacetone 0.6664g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, the α of one-tenth 0.6mol/L-thenoyltrifluoroacetone ethanolic soln;
3. prepare the 10 hendecenoic acid ethanolic soln
Take 10 hendecenoic acid 1.218mL ± 0.001mL, measure dehydrated alcohol 30.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the 10 hendecenoic acid ethanolic soln of 0.2mol/L;
4. prepare the sodium hydroxide ethanolic soln
Weighing sodium hydroxide 20.0g ± 0.1g, measure dehydrated alcohol 50.0mL ± 0.1mL, is placed in beaker, stirs 5min with agitator, becomes the sodium hydroxide ethanolic soln of 1mol/L;
5. prepare the terbium chloride ethanolic soln
Take terbium chloride 0.3733g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the terbium chloride ethanolic soln of 0.2mol/L;
6. prepare the anthranilic acid ethanolic soln
Take anthranilic acid 0.4114g ± 0.0001g, measure dehydrated alcohol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the anthranilic acid ethanolic soln of 0.6mol/L;
7. prepare the beryllium sulfate methanol solution
Take beryllium sulfate 0.3542g ± 0.0001g, measure anhydrous methanol 5.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become the beryllium sulfate methanol solution of 0.4mol/L;
8. prepare 2-(2-hydroxy phenyl) benzothiazole ethanolic soln
Take 2-(2-hydroxy phenyl) benzothiazole 0.4544g ± 0.0001g, measure anhydrous methanol 8.0mL ± 0.1mL, be placed in beaker, stir 5min with agitator, become 2-(2-hydroxy phenyl) the benzothiazole methanol solution of 0.25mol/L;
9. prepare sodium hydrate methanol solution
Weighing sodium hydroxide 20.0g ± 0.1g, measure anhydrous methanol 50.0mL ± 0.1mL, is placed in beaker, stirs 5min with agitator, becomes the sodium hydrate methanol solution of 1mol/L;
(2) prepare red light fluorescent powder
Prepare red light fluorescent powder and carry out in there-necked flask, complete in heating, stirring, dropping solution process;
1. there-necked flask is placed on electric heating cover, on there-necked flask top, inserts successively from left to right dropping funnel, agitator, pH meter;
2. 10 hendecenoic acid ethanolic soln 5mL is added in there-necked flask, opening electric heater, heating 10 hendecenoic acid ethanolic soln to 50 ℃ ± 2 ℃, turn on agitator, start to stir;
3. Europium trichloride ethanolic soln 5mL is added in dropping funnel, drip, rate of addition 1mL/min, stir on dropping limit, limit;
4. sodium hydroxide ethanolic soln 5mL is added in dropping funnel, drip, rate of addition 1mL/min, stir on dropping limit, limit, and regulating the pH value is 4.5-5.5, reaction times 30min;
5. α-thenoyltrifluoroacetone ethanolic soln 5mL is added in dropping funnel, drip, rate of addition 1mL/min, stir on dropping limit, limit, and regulating the pH value is 6.5-7.0;
6. continue reaction 180min;
7. stopped heating, stop stirring, and makes it with bottle is standing, be cooled to 25 ℃, and precipitation, obtains reaction soln;
8. suction filtration, be placed in the Büchner funnel on filter flask by reaction soln, uses the millipore filtration suction filtration, on filter membrane, obtains the product filter cake, and waste liquid is evacuated in filter flask;
9. washing, suction filtration, be placed in beaker by the product filter cake, adds dehydrated alcohol 100mL, agitator treating 5min; Then carry out suction filtration, washing, suction filtration repeat 5 times, obtain the product filter cake;
10. vacuum-drying, be placed in quartz container by the product filter cake, then is placed in vacuum drying oven dry, 60 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness-0.08Mpa, time of drying, 240min, obtained after drying: the europium red light fluorescent powder;
(3) prepare green light fluorescent powder
Prepare green light fluorescent powder and carry out in there-necked flask, complete in heating, stirring, dropping solution process;
1. there-necked flask is placed on electric heating cover, on there-necked flask top, inserts successively from left to right dropping funnel, agitator, pH meter;
2. 10 hendecenoic acid ethanolic soln 5mL is added in there-necked flask, opening electric heater, be heated to 50 ℃ ± 2 ℃, and turn on agitator stirs;
3. terbium chloride ethanolic soln 5mL is added in dropping funnel, drip, rate of addition 1mL/min, stir on dropping limit, limit, time 5min;
4. sodium hydroxide ethanolic soln 5mL is added in dropping funnel, and drip stirring, rate of addition 1mL/min, stir on dropping limit, limit, and regulating the pH value is 5.5-7.0;
5. anthranilic acid ethanolic soln 5mL is added in dropping funnel, and drip stirring, rate of addition 1mL/min, the pH value is 6.5-7.0;
6. continue reaction 300min;
7. stopped heating, stop stirring, and makes it with bottle is standing, be cooled to 25 ℃, and precipitation, obtains reaction soln;
8. suction filtration, be placed in the Büchner funnel on filter flask by reaction soln, uses the millipore filtration suction filtration, on filter membrane, obtains the product filter cake, and waste liquid is evacuated in filter flask;
9. washing, suction filtration, be placed in beaker by the product filter cake, adds dehydrated alcohol 100mL, agitator treating 5min; Then carry out suction filtration; Washing, suction filtration repeat 5 times, obtain the product filter cake;
10. vacuum-drying, be placed in quartz container by the product filter cake, then is placed in vacuum drying oven dry, 60 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness-0.08Mpa, time of drying, 240min, obtained after drying: the terbium green light fluorescent powder;
(4) prepare blue light fluorescent powder
Prepare blue light fluorescent powder and carry out in there-necked flask, complete in heating, stirring, dropping solution process;
1. there-necked flask is placed on electric heating cover, on there-necked flask top, inserts successively from left to right dropping funnel, agitator, pH meter;
2. by the 2-(2-hydroxy phenyl) benzothiazole methanol solution 5mL adds in there-necked flask; Opening electric heater, be heated to 50 ℃ ± 2 ℃; Turn on agitator stirs;
3. beryllium sulfate methanol solution 5mL is added in dropping funnel, and drip stirring, rate of addition 1mL/min, dropwise reaction time 30min;
4. α-methacrylic acid 0.0840mL ± 0.0001mL is added in dropping funnel, and add in there-necked flask, continue reaction 30min;
5. sodium hydrate methanol solution 5mL is added in dropping funnel, and drip, regulating the pH value is 8.0-9.0, yellow mercury oxide occurs, continues reaction 120min;
6. stopped heating, stop stirring, and makes it with bottle is standing, be cooled to 25 ℃, and precipitation, obtains reaction soln;
7. suction filtration, be placed in the Büchner funnel on filter flask by reaction soln, uses the millipore filtration suction filtration, on filter membrane, obtains the product filter cake, and waste liquid is evacuated in filter flask;
8. washing, suction filtration, be placed in beaker by the product filter cake, adds dehydrated alcohol 100mL, agitator treating 5min; Then carry out suction filtration; Washing, suction filtration repeat 5 times, obtain the product filter cake;
9. vacuum-drying, be placed in quartz container by the product filter cake, then is placed in vacuum drying oven dry, 60 ℃ ± 2 ℃ of drying temperatures, and vacuum tightness-0.08Mpa, time of drying, 240min, obtained after drying: the beryllium blue light fluorescent powder;
(5) prepare the monochromatic polymkeric substance of the Eu glowed
The monochromatic polymkeric substance of the Eu that preparation glows carries out in four-hole boiling flask, complete under heating, water-bath, stirring, nitrogen protection;
1. take europium red light fluorescent powder 0.0246g ± 0.0001g, methyl methacrylate 1.60mL ± 0.01mL, add in four-hole boiling flask;
Add initiator Diisopropyl azodicarboxylate 0.0074g ± 0.0001g;
Add solvent dimethyl sulfoxide (DMSO) 5.0mL ± 0.1mL;
Then four-hole boiling flask is carried out on the ultrasonic vibration instrument to ultrasonic vibration 30min, make its dissolving, become reaction soln;
2. four-hole boiling flask and reaction soln are placed on cleansing bath tub, water-bath water floods 4/5 of four-hole boiling flask volume, on four-hole boiling flask, inserts successively from left to right dropping funnel, agitator, pH meter, nitrogen tube;
3. to four-hole boiling flask input nitrogen, nitrogen input speed 25cm
3/ min;
4. heater, make the reaction soln temperature in four-hole boiling flask remain on 75 ℃ ± 2 ℃; Sustained reaction 48h;
5. while hot reaction soln is joined in 100mL methyl alcohol, generate gluey white precipitate, then with scissors, gluey white precipitate is shredded;
6. suction filtration, carry out suction filtration with millipore filtration, obtains the product filter cake;
7. filter cake is added in beaker, then add dimethyl sulfoxide (DMSO) 50mL, make its dissolving, then solution is poured in 100mL methyl alcohol and precipitated, repeat 5 times;
8. suction filtration, be placed in precipitated liquid on filter flask and use the millipore filtration suction filtration, obtains the product filter cake;
9. vacuum-drying, be placed in vacuum drying oven by the product filter cake dry, and drying temperature is 60 ℃ ± 2 ℃, vacuum tightness-0.08Mpa, and time of drying, 240min, obtained solid state powder after drying;
10. grind, sieve, solid state powder is ground with agate mortar, pestle, then with 600 eye mesh screens, sieve, grind, sieve and repeatedly carry out, the monochromatic polymer powder of the Eu that must glow;
(6) prepare the monochromatic polymkeric substance of Tb of green light
The monochromatic polymkeric substance of the Tb of preparation green light carries out in four-hole boiling flask, complete under heating, water-bath, stirring, nitrogen protection;
1. take terbium green light fluorescent powder 0.0654g ± 0.0001g, methyl methacrylate 1.60mL ± 0.01mL, add in four-hole boiling flask;
Add initiator Diisopropyl azodicarboxylate 0.0074g ± 0.0001g;
Add solvent dimethyl sulfoxide (DMSO) 5.0mL ± 0.1mL;
Then four-hole boiling flask is carried out on the ultrasonic vibration instrument to ultrasonic vibration 30min, make its dissolving, become reaction soln;
2. four-hole boiling flask and reaction soln are placed on cleansing bath tub, water-bath water floods 4/5 of four-hole boiling flask;
3. to four-hole boiling flask input nitrogen, nitrogen input speed 25cm
3/ min;
4. heater, make the reaction soln temperature in four-hole boiling flask remain on 75 ℃ ± 2 ℃; Continue reaction 48h;
5. while hot reaction soln is joined in 100mL methyl alcohol, generate gluey white precipitate, then with scissors, gluey white precipitate is shredded;
6. suction filtration, carry out suction filtration with millipore filtration, obtains the product filter cake;
7. filter cake is added in beaker, then add dimethyl sulfoxide (DMSO) 50mL, make its dissolving, then solution is poured in 100mL methyl alcohol and precipitated, repeat 5 times;
8. suction filtration, be placed in precipitated liquid on filter flask and use the millipore filtration suction filtration, obtains the product filter cake;
9. vacuum-drying, be placed in vacuum drying oven by the product filter cake dry, and drying temperature is 60 ℃ ± 2 ℃, vacuum tightness-0.08Mpa, and time of drying, 240min, obtained solid state powder after drying;
10. grind, sieve, solid state powder is ground with agate mortar, pestle, then with 600 eye mesh screens, sieve, grind, sieve and repeatedly carry out, obtain the monochromatic polymer powder of Tb of green light;
(7) prepare the monochromatic polymkeric substance of Be of blue light-emitting
The monochromatic polymkeric substance of Be for preparing blue light-emitting carries out in four-hole boiling flask, complete under heating, water-bath, stirring, nitrogen protection;
1. take beryllium blue light fluorescent powder 0.0160g ± 0.0001g, methyl methacrylate 1.60mL ± 0.01mL, add in four-hole boiling flask;
Add initiator Diisopropyl azodicarboxylate 0.0074g ± 0.0001g;
Add solvent dimethyl sulfoxide (DMSO) 5.0mL ± 0.1mL;
Then four-hole boiling flask is carried out on the ultrasonic vibration instrument to ultrasonic vibration 30min, make its dissolving, become reaction soln;
2. four-hole boiling flask and reaction soln are placed on cleansing bath tub, water-bath water floods 4/5 of four-hole boiling flask;
3. to four-hole boiling flask input nitrogen, nitrogen input speed 25cm
3/ min;
4. heater, make the reaction soln temperature in four-hole boiling flask remain on 75 ℃ ± 2 ℃, continues reaction 48h;
5. while hot reaction soln is joined in 100mL methyl alcohol, generate gluey white precipitate, then with scissors, gluey white precipitate is shredded;
6. suction filtration, carry out suction filtration with millipore filtration, obtains the product filter cake;
7. filter cake is added in beaker, then add dimethyl sulfoxide (DMSO) 50mL, make its dissolving, then solution is poured in 100mL methyl alcohol and precipitated, repeat 5 times;
8. suction filtration, be placed in precipitated liquid on filter flask and use the millipore filtration suction filtration, obtains the product filter cake;
9. vacuum-drying, be placed in vacuum drying oven by the product filter cake dry, and drying temperature is 60 ℃ ± 2 ℃, vacuum tightness-0.08Mpa, and time of drying, 240min, obtained solid state powder after drying;
10. grind, sieve, solid state powder is ground with agate mortar, pestle, then with 600 eye mesh screens, sieve, grind, sieve and repeatedly carry out, obtain the monochromatic polymer powder of Be of blue light-emitting;
(8) blend prepares white emitting fluorescent powder
Prepare white emitting fluorescent powder and be the monochromatic polymkeric substance of Eu, the monochromatic polymkeric substance of Tb, Be monochrome polymer-doped, through mixing, dissolving, precipitation, filtration, drying, obtain white emitting fluorescent powder;
1. it is red by the white light equilibrium principle, calculating the red, green, blue polymer ratio: green: indigo plant=1:1.38:0.46;
Take the monochromatic polymkeric substance 0.0100g ± 0.0001g of ruddiness Eu;
Take the monochromatic polymkeric substance 0.0138g ± 0.0001g of green glow Tb;
Take the monochromatic polymkeric substance 0.0046g ± 0.0001g of blue light Be;
Be placed in beaker, then add trichloromethane 10.0mL ± 0.1mL;
2. beaker is placed on the ultrasonic vibration instrument and vibrates 30min, make its dissolving;
3. measure methyl alcohol 100mL and add in beaker, standing 6h, make its precipitation;
4. suction filtration, be placed in precipitated liquid on filter flask, uses the millipore filtration suction filtration, obtains the product filter cake;
5. washing with alcohol, suction filtration, be placed in beaker by the product filter cake, adds ethanol 100mL agitator treating, suction filtration then, and washing, suction filtration repeat 3 times, obtain the product filter cake;
6. vacuum-drying, be placed in vacuum drying oven by the product filter cake after washing, suction filtration dry, and drying temperature is 60 ℃ ± 2 ℃, vacuum tightness-0.08Mpa, and time of drying, 240min, obtained white emitting fluorescent powder after drying;
(9) detect, analyze, characterize
Pattern, color and luster, composition, the chemical physics performance of white emitting fluorescent powder to preparation detects, analyzes, characterizes;
By fluorescence spectrophotometer, carry out fluorescent spectroscopy;
Conclusion: white emitting fluorescent powder is solid-state white powder, and particle diameter≤2000nm, chromaticity coordinates are x=0.3253, and y=0.3301, emit white light;
(10) product stores
White emitting fluorescent powder to preparation is stored in brown transparent Glass Containers, and airtight keeping in Dark Place wants waterproof, protection against the tide, anti-acid-alkali salt to corrode, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
2. the preparation method of a kind of RGB blend white emitting fluorescent powder according to claim 1, it is characterized in that: the preparation of ruddiness, green glow, blue light fluorescent powder, in there-necked flask, carrying out respectively, is to complete in the process of heating, stirring, adjusting potential of hydrogen;
The top of the first electric controller (1) is electric mantle (2), at the upper there-necked flask (3) of putting of electric mantle (2)
, the first dropping funnel (4) and first is set from left to right controls net (5), the first agitator (6), the first pH meter (7) on there-necked flask (3); The first display screen (9), the first pilot lamp (10), the first stirring modulator (11), the first Heating temperature modulator (12) are set on the front panel of the first electric controller 1.
3. the preparation method of a kind of RGB blend white emitting fluorescent powder according to claim 1, it is characterized in that: the preparation of ruddiness, green glow, the monochromatic polymkeric substance of blue light, in four-hole boiling flask, carry out respectively, complete under heating, stirring, water-bath, nitrogen protection;
The top of the second electric controller (13) is cleansing bath tub (14), the upper four-hole boiling flask (15) of putting of cleansing bath tub (14), on four-hole boiling flask (15) top by left-to-right the second dropping funnel (16) and the second control valve (17), the second agitator (18), the second pH meter (19), the nitrogen tube (20) of arranging; Nitrogen tube (20) connects nitrogen valve (21), nitrogengas cylinder (22); Second display screen (24), the second pilot lamp (25), the second stirring modulator (26), the second Heating temperature modulator (27) are set on the front panel of the second electric controller (13); In four-hole boiling flask (15), be reaction soln (23), nitrogen (28).
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| CN105238386B (en) * | 2014-08-18 | 2017-03-15 | 阜阳师范学院 | A kind of method of the fluorescent material for preparing rare earth doped complex |
| CN104693225B (en) * | 2015-02-11 | 2017-01-18 | 太原理工大学 | Preparation method of ternary complex capable of emitting bright green light |
| CN105001362A (en) * | 2015-07-30 | 2015-10-28 | 太原理工大学 | Rapid preparation method of blue-light-emitting fluorescent powder |
| CN105669728A (en) * | 2016-01-15 | 2016-06-15 | 太原理工大学 | Preparation method of bright yellow light-emitting europium complexes |
| CN105870302B (en) * | 2016-03-30 | 2019-01-29 | 深圳市聚飞光电股份有限公司 | A kind of packaging method of high colour gamut white light quanta point LED |
| CN108865114B (en) * | 2018-05-23 | 2021-02-12 | 太原理工大学 | Preparation method of white light macromolecular complex fluorescent powder containing europium terbium zinc |
| CN109181682A (en) * | 2018-09-17 | 2019-01-11 | 京东方科技集团股份有限公司 | White emitting fluorescent powder, preparation method and the LED light emission device using it |
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