CN106867519A - A kind of rear-earth-doped complex white light LED fluorescent powder and preparation method thereof - Google Patents
A kind of rear-earth-doped complex white light LED fluorescent powder and preparation method thereof Download PDFInfo
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- CN106867519A CN106867519A CN201710049918.9A CN201710049918A CN106867519A CN 106867519 A CN106867519 A CN 106867519A CN 201710049918 A CN201710049918 A CN 201710049918A CN 106867519 A CN106867519 A CN 106867519A
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- 239000000843 powder Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 20
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 239000003446 ligand Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 27
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- 229940113088 dimethylacetamide Drugs 0.000 claims description 10
- 239000012046 mixed solvent Substances 0.000 claims description 10
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims description 5
- 150000001732 carboxylic acid derivatives Chemical group 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910003317 GdCl3 Inorganic materials 0.000 abstract description 5
- MEANOSLIBWSCIT-UHFFFAOYSA-K gadolinium trichloride Chemical compound Cl[Gd](Cl)Cl MEANOSLIBWSCIT-UHFFFAOYSA-K 0.000 abstract description 5
- YIKSCQDJHCMVMK-UHFFFAOYSA-N Oxamide Chemical compound NC(=O)C(N)=O YIKSCQDJHCMVMK-UHFFFAOYSA-N 0.000 abstract 1
- GFISHBQNVWAVFU-UHFFFAOYSA-K terbium(iii) chloride Chemical compound Cl[Tb](Cl)Cl GFISHBQNVWAVFU-UHFFFAOYSA-K 0.000 abstract 1
- -1 rare earth ion Chemical class 0.000 description 15
- 150000002910 rare earth metals Chemical class 0.000 description 11
- 239000000463 material Substances 0.000 description 5
- 239000013110 organic ligand Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 0 C*(C)(C(C(*(C)(C)c1cc(C(O)=O)cc(C(O)=O)c1)=O)=O)c1cc(C(*)=O)cc(C(O)=O)c1 Chemical compound C*(C)(C(C(*(C)(C)c1cc(C(O)=O)cc(C(O)=O)c1)=O)=O)c1cc(C(*)=O)cc(C(O)=O)c1 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
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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
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
The present invention relates to a kind of rear-earth-doped complex white light LED fluorescent powder and preparation method thereof.A kind of rear-earth-doped complex white light LED fluorescent powder, chemical formula is { [Ln2(BDPO)1.5(DMA)3(H2O)]·5H2O}n.A kind of preparation method of rear-earth-doped complex white light LED fluorescent powder, including (1) configuration solvent；(2) respectively to adding EuCl in solvent3·6H2O、GdCl3·6H2O、TbCl3·6H2O, N, N ' two (M-phthalic acid) Oxamide Ligands, are uniformly mixing to obtain mixture；(3) then heating mixture is cooled to room temperature to 100~110 DEG C and constant temperature 70~80 hours, obtains product；(4) product that filtration step (3) is obtained, obtains colourless bulk crystals, as rear-earth-doped complex white light LED fluorescent powder.
Description
Technical field
The invention belongs to inorganic and materials chemistry scientific domain, more particularly to a kind of rear-earth-doped complex white light LEDs are glimmering
Light powder and preparation method thereof.
Background technology
Due to energy-conservation, environment-friendly, long lifespan and it is efficient the features such as, white light LEDs be widely used in display screen and
Illuminator, and be considered as forth generation light source.
In order to obtain with white luminous material, it is typically employed in material and introduces double-colored or three color strategies.Rare earth gold
Category ion has quantum yield higher, narrow and strong emission band, big stoke shift, the fluorescence lifetime of length and is not easy
Disturbed launch wavelength, therefore rare earth ion is the ideal chose for preparing the complex material with unique photoluminescent property.By
There is similar coordination environment in rare earth ion, so using different rare earth ions and during identical ligand reaction, usual
To with mutually isostructural complex.Therefore, not only different types of rare earth ion can be doped in same complex,
And the ratio that their contents in same complex can also add rare-earth salts by the control in synthesis is adjusted
Control.This means the fluorescence radiation color of rare earth compounding can be adjusted.Therefore, the different rare earth ions that adulterate arrive isomorphism
Turn into a kind of emerging and important method for preparing white fluorescence powder material in complex.However, presently relevant preparation method
And its material of correlation is also rare in the extreme, thus by different rare earth ions of adulterating prepare white light LED fluorescent powder turn into have weight
Want the work of meaning.
Because the f-f electro transfers that Laporte prohibits cause inefficient absorption, rare earth ion it is luminous very faint.Band
The organic ligand for having appropriate chromophores is seen as " antenna " or sensitizer to strengthen light absorpting ability and by antenna effect
Energy is transferred to rare earth ion from organic ligand, so as to strengthen the luminous of rare earth ion.Therefore, design contains big delocalization π
The organic ligand of electron-conjugated system for strengthen rare earth compounding fluorescence intensity for it is critical that.Preparing this hair
Organic ligand N, N '-two (the M-phthalic acid)-oxamides used in the complex of bright middle report has good flatness, shape
Into a typical big pi-electron conjugated system, impart the strong absorbing chromophores of part, thus be effectively sensitized it is rare earth luminous,
Successfully realize rear-earth-doped complex white light emission.
The content of the invention
Goal of the invention：The present invention makes improvement, i.e. the first object of the present invention for the problem that above-mentioned prior art is present
It is to disclose a kind of rear-earth-doped complex white light LED fluorescent powder.Second object of the present invention is to disclose a kind of rare earth to mix
The preparation method of miscellaneous complex white light LED fluorescent powder.
Technical scheme：A kind of rear-earth-doped complex white light LED fluorescent powder, chemical formula is { [Ln2(BDPO)1.5(DMA)3
(H2O)]·5H2O}n, in formula
Ln is three kinds of rare earth ion mixtures, consisting of Eu0.0855Gd0.6285Tb0.2860；
BDPO is to slough four N of carboxylic acid proton, N '-two (M-phthalic acid)-oxamides；
DMA is N, N '-dimethyl acetamide.
Further, the structural formula of BDPO is as follows：
A kind of preparation method of rear-earth-doped complex white light LED fluorescent powder, comprises the following steps：
(1) solvent is configured
Respectively by the DMAC N,N' dimethyl acetamide of 4000~4500 molar parts, the acetonitrile of 1700~2100 molar parts and 2600
The water of~3000 molar parts is added in closed container, well mixed to form mixed solvent；
(2) EuCl of 1 molar part is added in the mixed solvent for obtaining to step (1) respectively3·6H2O, 6 molar parts
GdCl3·6H2The TbCl of O, 3 molar parts3·6H2The N of O, 5 molar parts, N '-two (M-phthalic acid)-Oxamide Ligands, stirring
Mixture uniformly is obtained,
(3) mixture that heating stepses (2) are obtained is to 100~110 DEG C and constant temperature 70~80 hours, then with 0.1~0.3
DEG C/min speed be cooled to room temperature, obtain product；
(4) product that filtration step (3) is obtained, obtains colourless bulk crystals, as rear-earth-doped complex white light
LED fluorescent powder.
Further, the rear-earth-doped complex fluorescent powder of white light emission is three-dimensional frame structure, and it is excited in 390nm
Under, CIE coordinates are the coordinate value (0.33,0.33) of (0.34,0.33) closely pure white light, and quantum yield is 22.4%.
Beneficial effect：A kind of rear-earth-doped complex white light LED fluorescent powder disclosed by the invention and preparation method thereof has
Following beneficial effect：
1st, preparation process is simple, reaction condition are gentle；
2nd, the part for using is effectively absorbed by antenna effect and shifts energy, is sensitized rare earth luminescence, makes cooperation
Thing not only sends strong white light but also with quantum yield higher.
Brief description of the drawings
Fig. 1 is the rare earth Ln in a kind of rear-earth-doped complex white light LED fluorescent powder disclosed in this law3+The coordination ring of ion
Border figure；
Fig. 2 is that double-core cluster unit connects the layer structure figure for being formed in parallel with ac crystal faces by BDPO parts；
Fig. 3 is a kind of tomograph of rear-earth-doped complex white light LED fluorescent powder disclosed by the invention；
Fig. 4 is that a kind of rear-earth-doped complex white light LED fluorescent powder disclosed by the invention is glimmering under 390nm excitation wavelengths
Light spectrogram；
Fig. 5 is a kind of CIE coordinate diagrams of rear-earth-doped complex white light LED fluorescent powder disclosed by the invention.
Specific embodiment：
Specific embodiment of the invention is described in detail below.
Specific embodiment 1
A kind of rear-earth-doped complex white light LED fluorescent powder, chemical formula is { [Ln2(BDPO)1.5(DMA)3(H2O)]·
5H2O}n, in formula
Ln is three kinds of rare earth ion mixtures, consisting of Eu0.0855Gd0.6285Tb0.2860；
BDPO is to slough four N of carboxylic acid proton, N '-two (M-phthalic acid)-oxamides,
DMA is N, N '-dimethyl acetamide.
Further, the structural formula of BDPO is as follows：
A kind of preparation method of rear-earth-doped complex white light LED fluorescent powder, comprises the following steps：
(1) solvent is configured
The water of the DMAC N,N' dimethyl acetamide of 4000 molar parts, the acetonitrile of 1700 molar parts and 2600 molar parts is added respectively
Enter in closed container, be well mixed and form mixed solvent；
(2) EuCl of 1 molar part is added in the mixed solvent for obtaining to step (1) respectively3·6H2O, 6 molar parts
GdCl3·6H2The TbCl of O, 3 molar parts3·6H2The N of O, 5 molar parts, N '-two (M-phthalic acid)-Oxamide Ligands, stirring
Mixture uniformly is obtained,
(3) mixture that heating stepses (2) are obtained is to 100 DEG C and constant temperature 80 hours, then with 0.1 DEG C/min of speed
Room temperature is cooled to, product is obtained；
(4) product that filtration step (3) is obtained, obtains colourless bulk crystals, as rear-earth-doped complex white light
LED fluorescent powder.
Structure is described：
Structural characterization and parsing are carried out to obtained rear-earth-doped complex white light LED fluorescent powder, its structure cell and sky is determined
Between structure.
The complex belongs to monoclinic system, P21/ c space groups.Two rare earth Ln are included in one asymmetric cell3+From
Son, one and half BDPO parts and three DMAs of coordination.As shown in Figure 1, two rare earth ions have not
Same coordination environment：Its middle rare earth Ln1 with from four the six of BDPO parts carboxyl oxygen atoms, a hydrone and one
DMA molecular complexes, form the dodecahedron coordination environment of distortion；Rare earth Ln2 with come from four BDPO parts
Six carboxyl oxygen atoms and the coordination of two DMAs, form the dodecahedron coordination environment of distortion.Ln1 and
Ln2 forms double-core cluster unit by two carboxyl coordination bridgings with part, and double-core cluster unit interconnects structure by part
Into the layer structure parallel to ac crystal faces, as shown in Figure 2.Adjacent layer further extends to form three-dimensional knot by BDPO parts
Structure, as shown in Figure 3.
Fluorometric investigation：
As shown in figs. 4 and 5, the fluorescent emission of doped complexes can be accurate by adjusting the composition of three metal ion species
Ground regulation and control.On this basis, we optimize Eu3+、Gd3+And Tb3+The molar ratio of ion, has obtained rear-earth-doped complex white
Light LED fluorescent powder, determines that the composition of rare earth is Eu through inductively-coupled plasma spectrometer test0.0855Gd0.6285Tb0.2860.It is logical
The coordinate of the CIE coordinates (0.34,0.33) crossed under change excitation wavelength from 350 to 390nm, 390nm closely pure white light
Value (0.33,0.33), and its color temperature value is 5219K, is cool white light.The quantum of rear-earth-doped complex white light LED fluorescent powder is produced
Rate is 22.4%, higher than it is most of it has been reported that white light emission doped complexes.
Specific embodiment 2
A kind of rear-earth-doped complex white light LED fluorescent powder, chemical formula is { [Ln2(BDPO)1.5(DMA)3(H2O)]·
5H2O}n, in formula
Ln is three kinds of rare earth ion mixtures, consisting of Eu0.0855Gd0.6285Tb0.2860；
BDPO is to slough four N of carboxylic acid proton, N '-two (M-phthalic acid)-oxamides,
DMA is N, N '-dimethyl acetamide.
Further, the structural formula of BDPO is as follows：
A kind of preparation method of rear-earth-doped complex white light LED fluorescent powder, comprises the following steps：
(1) solvent is configured
The water of the DMAC N,N' dimethyl acetamide of 4300 molar parts, the acetonitrile of 1900 molar parts and 2800 molar parts is added respectively
Enter in closed container, be well mixed and form mixed solvent；
(2) EuCl of 1 molar part is added in the mixed solvent for obtaining to step (1) respectively3·6H2O, 6 molar parts
GdCl3·6H2The TbCl of O, 3 molar parts3·6H2The N of O, 5 molar parts, N '-two (M-phthalic acid)-Oxamide Ligands, stirring
Mixture uniformly is obtained,
(3) mixture that heating stepses (2) are obtained is to 110 DEG C and constant temperature 70 hours, then with 0.2 DEG C/min of speed
Room temperature is cooled to, product is obtained；
(4) product that filtration step (3) is obtained, obtains colourless bulk crystals, as rear-earth-doped complex white light
LED fluorescent powder.
Specific embodiment 3
A kind of rear-earth-doped complex white light LED fluorescent powder, chemical formula is { [Ln2(BDPO)1.5(DMA)3(H2O)]·
5H2O}n, in formula
Ln is three kinds of rare earth ion mixtures, consisting of Eu0.0855Gd0.6285Tb0.2860；
BDPO is to slough four N of carboxylic acid proton, N '-two (M-phthalic acid)-oxamides,
DMA is N, N '-dimethyl acetamide.
Further, the structural formula of BDPO is as follows：
A kind of preparation method of rear-earth-doped complex white light LED fluorescent powder, comprises the following steps：
(1) solvent is configured
The water of the DMAC N,N' dimethyl acetamide of 4500 molar parts, the acetonitrile of 2100 molar parts and 3000 molar parts is added respectively
Enter in closed container, be well mixed and form mixed solvent；
(2) EuCl of 1 molar part is added in the mixed solvent for obtaining to step (1) respectively3·6H2O, 6 molar parts
GdCl3·6H2The TbCl of O, 3 molar parts3·6H2The N of O, 0.5 molar part, N '-two (M-phthalic acid)-Oxamide Ligands, stir
Mix and uniformly obtain mixture,
(3) mixture that heating stepses (2) are obtained is to 105 DEG C and constant temperature 75 hours, then with 0.3 DEG C/min of speed
Room temperature is cooled to, product is obtained；
(4) product that filtration step (3) is obtained, obtains colourless bulk crystals, as rear-earth-doped complex white light
LED fluorescent powder.
Embodiments of the present invention are elaborated above.But the present invention is not limited to above-mentioned implementation method,
In the ken that art those of ordinary skill possesses, can also be done on the premise of present inventive concept is not departed from
Go out various change.
Claims (3)
1. a kind of rear-earth-doped complex white light LED fluorescent powder, it is characterised in that chemical formula is { [Ln2(BDPO)1.5(DMA)3
(H2O)]·5H2O}n, in formula
Ln is three kinds of rare earth ion mixtures, consisting of Eu0.0855Gd0.6285Tb0.2860；
BDPO is to slough four N of carboxylic acid proton, N '-two (M-phthalic acid)-oxamides；
DMA is N, N '-dimethyl acetamide.
2. a kind of rear-earth-doped complex white light LED fluorescent powder according to claim 1, it is characterised in that the knot of BDPO
Structure formula is as follows：
3. a kind of preparation method of rear-earth-doped complex white light LED fluorescent powder, it is characterised in that comprise the following steps：
(1) solvent is configured
Respectively by the DMAC N,N' dimethyl acetamide of 4000~4500 molar parts, the acetonitrile of 1700~2100 molar parts and 2600~
The water of 3000 molar parts is added in closed container, well mixed to form mixed solvent；
(2) EuCl of 1 molar part is added in the mixed solvent for obtaining to step (1) respectively3·6H2The GdCl of O, 6 molar parts3·
6H2The TbCl of O, 3 molar parts3·6H2The N of O, 5 molar parts, N '-two (M-phthalic acid)-Oxamide Ligands, are uniformly mixing to obtain
Mixture,
(3) mixture that heating stepses (2) are obtained is to 100~110 DEG C and constant temperature 70~80 hours, then with 0.1~0.3 DEG C/
The speed of minute is cooled to room temperature, obtains product；
(4) product that filtration step (3) is obtained, obtains colourless bulk crystals, and as rear-earth-doped complex white light LEDs are glimmering
Light powder.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107382767A (en) * | 2017-08-10 | 2017-11-24 | 西北大学 | A kind of metal organic framework compound and its preparation method and application |
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| CN107382767A (en) * | 2017-08-10 | 2017-11-24 | 西北大学 | A kind of metal organic framework compound and its preparation method and application |
| CN107382767B (en) * | 2017-08-10 | 2019-04-23 | 西北大学 | A kind of metal organic framework compound and its preparation method and application |
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