CN106905956A - A kind of white light LEDs yellow fluorescent material and its preparation method and application - Google Patents
A kind of white light LEDs yellow fluorescent material and its preparation method and application Download PDFInfo
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- CN106905956A CN106905956A CN201710115783.1A CN201710115783A CN106905956A CN 106905956 A CN106905956 A CN 106905956A CN 201710115783 A CN201710115783 A CN 201710115783A CN 106905956 A CN106905956 A CN 106905956A
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- 239000000463 material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 150000001412 amines Chemical class 0.000 claims abstract description 13
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 12
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- SBBQDUFLZGOASY-OWOJBTEDSA-N 4-[(e)-2-(4-carboxyphenyl)ethenyl]benzoic acid Chemical class C1=CC(C(=O)O)=CC=C1\C=C\C1=CC=C(C(O)=O)C=C1 SBBQDUFLZGOASY-OWOJBTEDSA-N 0.000 claims abstract description 8
- 101100046775 Arabidopsis thaliana TPPA gene Proteins 0.000 claims abstract description 8
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011701 zinc Substances 0.000 claims abstract description 6
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims description 22
- 238000005352 clarification Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- SPURMHFLEKVAAS-UHFFFAOYSA-N 1-docosene Chemical compound CCCCCCCCCCCCCCCCCCCCC=C SPURMHFLEKVAAS-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- 238000006862 quantum yield reaction Methods 0.000 abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 10
- 239000012621 metal-organic framework Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000425573 Talanes Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 238000002447 crystallographic data Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- OONPLQJHBJXVBP-UHFFFAOYSA-N 3-(2-phenylethenyl)phthalic acid Chemical compound OC(=O)C1=CC=CC(C=CC=2C=CC=CC=2)=C1C(O)=O OONPLQJHBJXVBP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241001085205 Prenanthella exigua Species 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- YSGZPEILUZVKDO-UHFFFAOYSA-N [F].C1(=CC=CC=C1)N(C1=CC=CC=C1)C1=CC=CC=C1 Chemical group [F].C1(=CC=CC=C1)N(C1=CC=CC=C1)C1=CC=CC=C1 YSGZPEILUZVKDO-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229940125904 compound 1 Drugs 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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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
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
- C07C63/33—Polycyclic acids
- C07C63/331—Polycyclic acids with all carboxyl groups bound to non-condensed rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/24—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D213/36—Radicals substituted by singly-bound nitrogen atoms
- C07D213/38—Radicals substituted by singly-bound nitrogen atoms having only hydrogen or hydrocarbon radicals attached to the substituent nitrogen atom
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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
- 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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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Computer Hardware Design (AREA)
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Abstract
A kind of white light LEDs yellow fluorescent material and preparation method thereof, its chemical formula is：Zn4(TPPA)2(sdc)3(NO3)2；Wherein TPPA represents three [(4 pyridine radicals) phenyl] amine, sdc represents 4,4' stilbenedicarboxylicacid acids, by zinc nitrate hexahydrate, three [(4 pyridine radicals) phenyl] amine, 4,4' stilbenedicarboxylicacid acids mix, and add N, N dimethylformamides and acetonitrile and stir, it is fitted into resistant to elevated temperatures vial, isothermal reaction 48h obtains product at 85 DEG C.The material can launch strong gold-tinted and with good fluorescence quantum yield, have potential application value in white light LEDs field.
Description
Technical field
The invention belongs to luminescent metal organic framework materials field, it is related to a kind of based on three [(4- pyridine radicals) phenyl] amine
Part, with Zn2+, the metal organic framework compound that 4,4'- stilbenedicarboxylicacid acids are self-assembly of and preparation method thereof, and
Using the application of the compound fluorescent characteristic.
Background technology
LED (Light EmittingDiode) as a kind of new luminescent device, with low current, luminescent effect it is fast,
The advantages of stable performance, small volume, long lifespan, and without harmful mercury metal, do not pollute the environment, gradually develop at present
Principal light source mode as various illuminations, is all significant to aspects such as energy-saving and environmental protection, improvement people's qualities of life
And economic worth.
Current white LED light source realizes that white light mainly has following three kinds of methods：1. three kinds of hairs of color of red, green, blue are used
Optical diode produces white light；2. blue-ray LED coating yellow fluorescent powder obtains white light；3. using near ultraviolet, ultraviolet LED excite it is red,
Green, blue phosphor, carries out three coloured light mixing and obtains white light.The disadvantage of first method is that price is higher is unfavorable for commodity
Change development；Burst of ultraviolel is used in the third method, not only energy comparatively high consumption, and be unfavorable for environmental protection, especially can be to human eye
Produce serious harm；In view of these aspects, second method has potential advantage.Commercial fluorescent material major part is dilute now
The oxide or nitride of earth metal such as europium, terbium, yttrium etc., rare earth are extremely precious and in recent years as non-renewable resource
Price goes up all the way, therefore, the fluorescent material for finding available abundant element preparation is significant.
The fluorine-triphenylamine structure stabilization containing relatively strong blueness effect group that the present invention chooses, is a kind of important hole-conductive point
Son, there is fluorescence property and photoluminescence efficiency higher.Three (4- (pyridine radicals)-phenyl) amine with trianilino group as core are made
It is main part, and 4,4'- stilbenedicarboxylicacid acid and zinc nitrate hexahydrate, obtains having by solvent structure good blue
Light activated gold-tinted metal-organic framework materials, compare, by with commercial YAG (Ce) material it can be found that the material is accorded with substantially
Conjunction prepares the technical requirements of white light LEDs.
The content of the invention
The technical problem of solution：The present invention provides a kind of white light LEDs yellow fluorescent material and its preparation method and application,
By reasonably changing reaction dissolvent system, to prepare the luminophor with good nature, this is further expanded and has lighted
The breadth and depth of material.
Technical scheme：A kind of white light LEDs yellow fluorescent material, the chemical formula of the compound is：Zn4(TPPA)2
(sdc)3(NO3)2；Wherein, wherein TPPA represents three [(4- pyridine radicals) phenyl] amine, and sdc represents 4,4'- stilbenedicarboxylicacid acids,
Its structural formula is
The preparation method of white light LEDs yellow fluorescent material, preparation process is：Weigh in proportion zinc nitrate hexahydrate 0.02~
0.05mmol, three [(4- pyridine radicals) phenyl] amine 0.02~0.05mmol, 4,4'- 0.02~0.05mmol of stilbenedicarboxylicacid acid
It is added in reaction vessel, adds 2~5mLN, dinethylformamide and 1~2.5mL acetonitriles, ultrasonic dissolution, treats that solution becomes
Clarification, reaction vessel is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, room temperature is down to naturally, obtains yellow block
Crystal, filtering obtains final product product.
Preferably, zinc nitrate hexahydrate 0.02mmol is weighed in proportion, three [(4- pyridine radicals) phenyl] amine 0.02mmol, 4,
4'- stilbenedicarboxylicacid acids 0.02mmol is added in reaction vessel, adds 2mL DMFs and 1mL second
Nitrile, ultrasonic dissolution, solution becomes clarification, reaction vessel is put into thermostatic drying chamber, Temperature fall after isothermal reaction 48h at 85 DEG C
Yellow bulk crystals are obtained, filtering obtains final product product.
Application of the above-mentioned yellow fluorescent material in white light LEDs material is prepared.
A kind of white light LEDs material, is obtained by above-mentioned yellow fluorescent material.
Beneficial effect：Triphenylamine organic ligand and zinc metal ion are carried out self assembly by the present invention, are prepared for a kind of yellow
Fluorescent material.Overcome in white light emitting material mainly using expensive, environmental hazard rare earth metal the shortcomings of.The compound
Synthetic method is simple, and favorable reproducibility is easy to operate, safety, and for us, purposefully synthesis has good fluorescence performance from now on
Functional material give reference.Fluorescence property shows that the compound can launch gold-tinted in the case where blue light is excited, in white light LEDs material
Material aspect has broad application prospects.
Brief description of the drawings
Fig. 1 is the one-dimensional channels schematic diagram of embodiment 1；
Fig. 2 is the topological diagram of embodiment 1；
Fig. 3 is powder X-ray RD (PXRD) diffraction spectrogram of embodiment 1；
Fig. 4 is the fluorescence spectra of embodiment 1；
Fig. 5 is chromaticity diagram (CIE) (λ of embodiment 1ex=365nm)；
Fig. 6 is thermogravimetric (TG) curve spectrogram of embodiment 1；
Fig. 7 is infrared (IR) spectrogram of embodiment 1；
Fig. 8 is LED component figure prepared by embodiment 1.
Specific embodiment
Technical scheme is described in detail with reference to embodiment, be not meant to limitation of the present invention.
All reagents are all commercially available below, and zinc nitrate hexahydrate, acetonitrile are purchased from Chinese medicines group, DMF
(DMF) then it is purchased from Shanghai Aladdin reagent Co., Ltd.
Additionally need be illustrated be：
Powder x-ray diffraction test condition：Tube voltage 40kV, tube current 10mA, CuK α are radiated, and wavelength isSurvey
5-50 ° of angular range of examination, 0.02 ° of step-length, 6 °/min of sweep speed；TG/DTA test conditions：Under nitrogen protection, calefactive interzone
From room temperature to 800 DEG C or so, heating rate is 10 DEG C of min-1；Infrared spectrum measurement uses Nicolet FT-1703X infrared lights
Spectrometer (KBr compressing tablets), test scope is in 4000cm-1~500cm-1Between carry out.Fluorescence analysis test is used
Spectrofluorometer FS5 XRFs；The test of solid fluorescence quantum yield uses Hamamatsu
Multichannel analyzer c10027 instruments.
Embodiment 1
Compound Zn4(TPPA)2(sdc)3(NO3)2Synthesis
Accurately weigh zinc nitrate hexahydrate 0.02mmol, three [(4- pyridine radicals) phenyl] amine 0.02mmol, 4,4'- talan
Dicarboxylic acids 0.02mmol is added in reaction vessel, adds 2mLN, dinethylformamide and 1mL acetonitriles, and ultrasonic dissolution is molten
Liquid becomes clarification, and reaction vessel is put into thermostatic drying chamber, and Temperature fall obtains the block crystalline substance of yellow after isothermal reaction 48h at 85 DEG C
Body, filtering obtains final product product.Yield：45%, infrared (IR)：3433(m),1652(s),1605(s),1390(s),1083(w),
812(w)。
Embodiment 2
Crystal structure determination to implementing compound 1:
The monocrystalline of suitable size is chosen under the microscope, and point diffraction is collected on Bruker SMARTAPEX CCD detection instrument
Data.At a temperature of 173K, with epoxide-resin glue by single crystal sticky on glass fiber, use graphite monochromatised Mo K α radiation
(λ=0.071073nm) ray is collected.Diffracted intensity data are through the Lp factors and empirical absorption correction.The crystal knot of compound
Structure is analyzed and calculated and completed with SHELXL programs, and has made absorption or extinction correction with SADABS.Non-hydrogen atom coordinate is poor
Fourier synthesis is obtained, and complete matrix least square method amendment has been carried out to whole non-hydrogen atom coordinates and anisotropy thermal parameter,
Hydrogen atom is obtained with theoretical method of hydrotreating, and participates in structure-factor.Relevant crystallographic data is shown in Table 1.One-dimensional channels are shown in figure
1, topological structure is shown in Fig. 2.
Table 1 is compound Zn4(TPPA)2(sdc)3(NO3)2The crystallographic data of sum
For powder X-ray RD (PXRD) diffraction test of the metal organic framework compound prepared by above-described embodiment 1：
Fig. 3 is the crystalline substance of the PXRD diffraction test spectrogram with embodiment 1 of the metal organic framework compound prepared by the present invention
Volume data simulates PXRD spectrogram comparison diagrams, it can be seen that the simulated diffraction peak of prepared compound is measured with actual experiment in figure
It is fine that diffraction maximum is contrasted, and illustrates that compound has phase purity very high.
For the fluorescence property test of the metal organic framework compound obtained by above-described embodiment 1：
Fig. 4 is the fluorescence property test spectrogram of the metal organic framework compound prepared by embodiment 1, from fluorescence spectrum
In figure it can be seen that its maximum emission peak position is 527nm；And solid fluorescence quantum yield test result shows embodiment 1
Fluorescence quantum yield is up to 20.5% (λex=365nm)；
Fig. 5 is the chromaticity diagram of the metal organic framework compound prepared by embodiment 1, its chromaticity diagram coordinate be (0.46,
0.52)(λex=365nm), it can be seen that the compound Yellow light-emitting low temperature in figure.
Fig. 6 is for the thermogravimetric analysis to the compound in embodiment 1 is characterized, as can be seen that three from thermogravimetric analysis (TGA)
Individual compound suffers from stability very high.But with the rising of temperature, at 400 DEG C or so, the structure of compound starts to collapse
Collapse and decompose.
It is the IR Characterization figure to the compound in embodiment 1 that Fig. 7 is.
Fig. 8 is after being de-gassed dried process to the compound that embodiment 1 is obtained, to be applied in the LED lamp bead of blue light-emitting
Face, after switching on power, sends bright white light.
Embodiment 3
Accurately weigh zinc nitrate hexahydrate 0.05mmol, three [(4- pyridine radicals) phenyl] amine 0.05mmol, 4,4'- talan
Dicarboxylic acids 0.05mmol is added in reaction vessel, adds 5mL DMFs and 2.5mL acetonitriles, and ultrasound is molten
Solution, solution becomes clarification, and reaction vessel is put into thermostatic drying chamber, is naturally cooling to room temperature, mistake at 85 DEG C after isothermal reaction 48h
Above-mentioned yellow fluorescent material is obtained after filter.
Embodiment 4
Zinc nitrate hexahydrate 0.03mmol, three [(4- pyridine radicals) phenyl] amine 0.04mmol, 4,4'- hexichol second are weighed in proportion
Docosene dicarboxylic acid 0.03mmol is added in reaction vessel, adds 3mL DMFs and 2mL acetonitriles, and ultrasound is molten
Solution, treats that solution becomes clarification, and reaction vessel is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, room temperature is down to naturally,
Yellow bulk crystals are obtained, filtering obtains final product product.
Claims (5)
1. a kind of white light LEDs yellow fluorescent material, it is characterised in that：The chemical formula of the compound is：Zn4(TPPA)2
(sdc)3(NO3)2；Wherein, wherein TPPA represents three [(4- pyridine radicals) phenyl] amine, and sdc represents 4,4'- stilbenedicarboxylicacid acids,
Its structural formula is
2. the preparation method of white light LEDs yellow fluorescent material described in claim 1, it is characterised in that preparation process is：By than
Example weighs zinc nitrate hexahydrate 0.02~0.05mmol, three [(4- pyridine radicals) phenyl] 0.02~0.05mmol of amine, 4,4'- hexichol second
0.02~0.05mmol of docosene dicarboxylic acid is added in reaction vessel, adds 2~5mLN, dinethylformamide and 1~2.5mL
Acetonitrile, ultrasonic dissolution treats that solution becomes clarification, and reaction vessel is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, from
Room temperature is so down to, yellow bulk crystals are obtained, filtering obtains final product product.
3. the preparation method of white light LEDs yellow fluorescent material according to claim 2, it is characterised in that weigh in proportion
Zinc nitrate hexahydrate 0.02mmol, three [(4- pyridine radicals) phenyl] amine 0.02mmol, 4,4'- stilbenedicarboxylicacid acid 0.02mmol add
Enter in reaction vessel, add 2mL DMFs and 1mL acetonitriles, ultrasonic dissolution, solution becomes clarification, will react
Container is put into thermostatic drying chamber, and Temperature fall obtains yellow bulk crystals after isothermal reaction 48h at 85 DEG C, and filtering obtains final product product
Thing.
4. application of the yellow fluorescent material described in claim 1 in white light LEDs material is prepared.
5. a kind of white light LEDs material, it is characterised in that be obtained as yellow fluorescent material described in claim 1.
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| CN108794759A (en) * | 2018-08-27 | 2018-11-13 | 江苏科技大学 | A kind of zinc-base luminescent metal organic framework material and its preparation method and application |
| CN109438721A (en) * | 2018-11-15 | 2019-03-08 | 江苏科技大学 | A kind of cadmium base luminescent metal organic framework material and its preparation method and application with high-fluorescence quantum yield |
| CN116082659A (en) * | 2023-02-28 | 2023-05-09 | 苏州芼孚士科技有限公司 | MOF-derived high-pore carbon aerogel and application thereof in super capacitor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794759A (en) * | 2018-08-27 | 2018-11-13 | 江苏科技大学 | A kind of zinc-base luminescent metal organic framework material and its preparation method and application |
| CN109438721A (en) * | 2018-11-15 | 2019-03-08 | 江苏科技大学 | A kind of cadmium base luminescent metal organic framework material and its preparation method and application with high-fluorescence quantum yield |
| CN116082659A (en) * | 2023-02-28 | 2023-05-09 | 苏州芼孚士科技有限公司 | MOF-derived high-pore carbon aerogel and application thereof in super capacitor |
| CN116082659B (en) * | 2023-02-28 | 2023-10-20 | 苏州芼孚士科技有限公司 | MOF-derived high-pore carbon aerogel and application thereof in super capacitor |
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