CN106995696A - A kind of zinc-base luminescent metal organic framework material and its preparation method and application - Google Patents
A kind of zinc-base luminescent metal organic framework material and its preparation method and application Download PDFInfo
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- CN106995696A CN106995696A CN201710115821.3A CN201710115821A CN106995696A CN 106995696 A CN106995696 A CN 106995696A CN 201710115821 A CN201710115821 A CN 201710115821A CN 106995696 A CN106995696 A CN 106995696A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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Abstract
A kind of zinc-base luminescent metal organic framework material and its preparation method and application, its chemical formula is：Zn (TPPA) (ndc), wherein TPPA represents three [(4 pyridine radicals) phenyl] amine, and ndc represents 2,6 naphthalene dicarboxylic acids, by zinc nitrate hexahydrate, three [(4 pyridine radicals) phenyl] amine, the mixing of 2,6 naphthalene dicarboxylic acids, add N, N dimethylformamides are simultaneously stirred, and are fitted into resistant to elevated temperatures vial, and it is the luminescent metal organic framework compounds that isothermal reaction 48h, which obtains product, at 85 DEG C.The present invention 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 material field, it is related to one kind based on three [(4- pyridine radicals) phenyl] amine
Part, with Zn2+, the metal organic framework compound that 2,6- naphthalene dicarboxylic acids are self-assembly of and preparation method thereof, and utilization should
Application in terms of compound fluorescent characteristic.
Background technology
LED (Light Emitting Diode) is as a kind of new luminescent device, with low current, luminescent effect
Hurry up, performance stabilization, small volume, long lifespan the advantages of, and without harmful mercury metal, do not pollute the environment, gradually at present
Develop into the principal light source mode of various illuminations, it is great to all having in terms of energy-saving and environmental protection, improvement people's quality of life
Meaning and economic value.Current white LED light source realizes one of main path of white light, just can be by blue-ray LED coating
The mode of yellow fluorescent powder obtains white light.Commercial fluorescent material is largely the oxide of rare earth metal such as europium, terbium, yttrium etc. now
Or nitride, rare earth is extremely precious as non-renewable resource, and price goes up all the way in recent years, and therefore, searching can
The fluorescent material prepared with abundant element is significant.
There is the metal-organic framework materials material of good luminous property nearly ten years, because of its porous, rich and varied
The characteristics of luminescence, the application prospect of great potential, and the MOFs materials with specific lighting function are built, it can be widely applied to white
Light-emitting material, small molecule detection, explosive detection, the numerous areas such as pH detections and TEMP.Attract numerous scientific researches
The extensive concern of worker.
The fluorine-triphenylamine structure containing relatively strong blue effect group that the present invention chooses is stable, is a kind of important hole-conductive point
Son, there is higher fluorescence property and photoluminescence efficiency.Three (4- (pyridine radicals)-phenyl) amine by core of trianilino group are made
For main part, and 2,6- naphthalene dicarboxylic acids and zinc nitrate hexahydrate, obtain exciting with good blue light by solvent structure
Gold-tinted metal-organic framework materials, by being compared with commercial YAG (Ce) material, it can be found that the material substantially conform to prepare
The technical requirements of white light LEDs.
The content of the invention
The technical problem of solution：The present invention provides a kind of zinc-base luminescent metal organic framework material and preparation method and its should
With.And by reasonably changing reaction dissolvent system, to prepare the luminophor with good nature, further expanded this
The breadth and depth of luminescent material.
Technical scheme：A kind of zinc-base luminescent metal organic framework material, the chemical formula of the compound is：Zn(TPPA)
(ndc), wherein TPPA represents three [(4- pyridine radicals) phenyl] amine, and ndc represents 2,6- naphthalene dicarboxylic acids, and its structural formula is：
The preparation method of above-mentioned zinc-base luminescent metal organic framework material, preparation process is：In proportion, six water nitric acid are weighed
The naphthalene dicarboxylic acids of zinc 0.02~0.05mmol, three [(4- pyridine radicals) phenyl] amine 0.02~0.05mmol, 2,6- 0.02~
0.05mmol is added in reaction vessel, adds 1~5mL DMFs, and 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, light yellow bulk is obtained brilliant
Body, filtering produces product.
It is preferred that, in proportion, weigh zinc nitrate hexahydrate 0.02mmol, three [(4- pyridine radicals) phenyl] amine 0.02mmol, 2,
6- naphthalene dicarboxylic acids 0.02mmol is added in reaction vessel, adds 2.5mL DMFs, and ultrasonic dissolution treats molten
Liquid becomes clarification, and reaction vessel is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, and room temperature is down to naturally, obtains pale yellow
Color bulk crystals, filtering produces product.
Application of the above-mentioned zinc-base luminescent metal organic framework material in white light LEDs material is prepared.
A kind of white light LEDs material, is made by above-mentioned zinc-base luminescent metal organic framework material.
Beneficial effect：Triphenylamine organic ligand and zinc metal ion are carried out self assembly by the present invention, are prepared for Yellow light-emitting low temperature
Metal organic framework compound.By the fluorescent characteristic of organic ligand, it is incorporated into well among Inorganic-Organic Hybrid Material, gram
The shortcomings of having taken in white light emitting material mainly using expensive, environmental hazard rare earth metal.The synthetic method letter of the compound
Single, favorable reproducibility is easy to operate, safety, and for us, purposefully synthesis has the feature material of good fluorescence performance from now on
Material gives reference.Fluorescence property shows that the compound can launch gold-tinted in the case where blue light is excited, and has in terms of white light LEDs material
Wide application prospect.
Brief description of the drawings
Fig. 1 is the topological diagram of embodiment 1；
Fig. 2 is powder X-ray RD (PXRD) diffraction spectrogram of embodiment 1；
Fig. 3 is the fluorescence spectra of embodiment 1；
Fig. 4 is chromaticity diagram (CIE) (λ of embodiment 1ex=365nm)；
Fig. 5 is thermogravimetric (TG) curve spectrogram of embodiment 1；
Fig. 6 is infrared (IR) spectrogram of embodiment 1；
Fig. 7 is the LED component figure of the preparation of embodiment 1.
Embodiment
Technical scheme is described in detail with reference to embodiment, is not meant to limitation of the present invention.
All reagents are all commercially available below, and zinc nitrate hexahydrate is purchased from Chinese medicines group, and DMF (DMF) is then
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
Try 5-50 ° of angular range, 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 tablettings), 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 Zn (TPPA) (ndc) synthesis
Accurately weigh zinc nitrate hexahydrate 0.02mmol, three [(4- pyridine radicals) phenyl] amine 0.02mmol, 2,6- naphthalene dicarboxylic acids
0.02mmol is added in reaction vessel, adds 2.5mL DMFs, and 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, light yellow bulk is obtained brilliant
Body, filtering produces product.Yield：55%, infrared (IR)：3436(m),1667(s),1601(s),1492(s),1350(s),
1081(w),807(m),651(w)。
Embodiment 2
Crystal structure determination to the compound of embodiment 1:
The monocrystalline of suitable size is chosen under the microscope, and diffraction is collected on Bruker SMART APEX CCD detection instrument
Point 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.Chemical combination
The crystal structure analysis and calculating of thing are completed with SHELXL programs, and have made absorption or extinction correction with SADABS.Non-hydrogen atom
Coordinate difference Fourier synthesis is obtained, and complete matrix least square has been carried out to whole non-hydrogen atom coordinates and anisotropy thermal parameter
Method amendment, hydrogen atom is obtained with theoretical method of hydrotreating, and participates in structure-factor.Relevant crystallographic data is shown in Table 1.Topology knot
Structure is shown in Fig. 1.
Table 1 is compound Zn (TPPA) (ndc) crystallographic data
For powder X-ray RD (PXRD) diffraction test of the metal organic framework compound prepared by above-described embodiment 1：
Fig. 2 is the PXRD diffraction test spectrogram and the crystal of embodiment 1 of metal organic framework compound prepared by the present invention
Digital simulation PXRD spectrogram comparison diagrams, the simulated diffraction peak of the compound prepared by it can be seen from the figure that is measured with actual experiment to spread out
The fine of peak contrast is penetrated, illustrates that compound has very high phase purity.
For the fluorescence property test of the metal organic framework compound obtained by above-described embodiment 1：
Fig. 3 is the fluorescence property test spectrogram of the metal organic framework compound prepared by embodiment 1, from fluorescence spectra
In it can be seen that its maximum emission peak position be 538nm；And solid fluorescence quantum yield test result shows the glimmering of embodiment 1
Quantum yield is up to 36.6% (λex=365nm)；
Fig. 4 is the chromaticity diagram of the metal organic framework compound prepared by embodiment 1, and its chromaticity diagram coordinate is respectively
(0.35,0.40)(λex=365nm), the it can be seen from the figure that compound Yellow light-emitting low temperature.
Fig. 5 is to be characterized to the thermogravimetric analysis of the compound in embodiment 1, as can be seen that should from thermogravimetric analysis (TGA)
Compound suffers from very high stability.But with the rise of temperature, at 400 DEG C or so, the structure of compound starts to cave in
And decompose.
Fig. 6 is for the IR Characterization to the compound in embodiment 1.
Fig. 7 is that the compound that embodiment 1 is obtained is de-gassed after drying process 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, 2,6- naphthalene dicarboxylic acids
0.05mmol is added in reaction vessel, adds 5mL DMFs, and ultrasonic dissolution treats that solution becomes clarification, will
Reaction vessel is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, and room temperature is down to naturally, obtains light yellow bulk crystal,
Filtering produces above-mentioned metal-organic framework materials.
Embodiment 4
Weigh zinc nitrate hexahydrate 0.03mmol, three [(4- pyridine radicals) phenyl] amine 0.03mmol, 2,6- naphthalene dicarboxylic acids
0.03mmol is added in reaction vessel, adds 3mL DMFs, and ultrasonic dissolution treats that solution becomes clarification, will
Reaction vessel is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, and room temperature is down to naturally, obtains light yellow bulk crystal,
Filtering produces product.
Claims (5)
1. a kind of zinc-base luminescent metal organic framework material, it is characterised in that：The chemical formula of the compound is：Zn(TPPA)
(ndc), wherein TPPA represents three [(4- pyridine radicals) phenyl] amine, and ndc represents 2,6- naphthalene dicarboxylic acids, and its structural formula is：
2. a kind of preparation method of zinc-base luminescent metal organic framework material described in claim 1, it is characterised in that preparation process
For：In proportion, zinc nitrate hexahydrate 0.02~0.05mmol is weighed, three [(4- pyridine radicals) phenyl] amine 0.02~0.05mmol, 2,
0.02~0.05mmol of 6- naphthalene dicarboxylic acids is added in reaction vessel, adds 1~5mL DMFs, and ultrasound is molten
Solution, 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,
Light yellow bulk crystal is obtained, filtering produces product.
3. the preparation method of a kind of zinc-base luminescent metal organic framework material according to claim 2, it is characterised in that press
Ratio, weighs zinc nitrate hexahydrate 0.02mmol, three [(4- pyridine radicals) phenyl] amine 0.02mmol, 2,6- naphthalene dicarboxylic acids 0.02mmol
It is added in reaction vessel, adds 2.5mL DMFs, ultrasonic dissolution treats that solution becomes clarification, reaction is held
Device is put into thermostatic drying chamber, at 85 DEG C after isothermal reaction 48h, and room temperature is down to naturally, obtains light yellow bulk crystal, and filtering is
Obtain product.
4. application of the zinc-base luminescent metal organic framework material in white light LEDs material is prepared described in claim 1.
5. a kind of white light LEDs material, it is characterised in that be made as zinc-base luminescent metal organic framework material described in claim 1.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587607A (en) * | 2018-05-18 | 2018-09-28 | 陕西科技大学 | The luminescent metal organic framework material and its preparation method and application detected for Thiocyanate ion in water |
| 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 |
| CN110283330A (en) * | 2019-06-28 | 2019-09-27 | 江苏科技大学 | Based on zinc-base luminescent metal organic framework material and its preparation method and application |
| CN114507355A (en) * | 2022-01-14 | 2022-05-17 | 江苏科技大学 | Zinc-based triazole luminescent material and preparation method and application thereof |
| 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 (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587607A (en) * | 2018-05-18 | 2018-09-28 | 陕西科技大学 | The luminescent metal organic framework material and its preparation method and application detected for Thiocyanate ion in water |
| CN108587607B (en) * | 2018-05-18 | 2020-10-27 | 陕西科技大学 | Luminescent metal organic framework material for detecting thiocyanate ions in water and preparation method and application thereof |
| 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 |
| CN110283330A (en) * | 2019-06-28 | 2019-09-27 | 江苏科技大学 | Based on zinc-base luminescent metal organic framework material and its preparation method and application |
| CN110283330B (en) * | 2019-06-28 | 2022-01-28 | 江苏科技大学 | Zinc-based luminescent metal organic framework material and preparation method and application thereof |
| CN114507355A (en) * | 2022-01-14 | 2022-05-17 | 江苏科技大学 | Zinc-based triazole luminescent material and preparation method and application thereof |
| 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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Application publication date: 20170801 |