CN105441064A - White light material EuxDy1-xZn2L2(Hfac)6 and preparation method thereof - Google Patents
White light material EuxDy1-xZn2L2(Hfac)6 and preparation method thereof Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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Abstract
The invention discloses a white light material EuxDy1-xZn2L2(Hfac)6 and a preparation method thereof, and in particular relates to a white light material and a preparation method thereof. The invention aims to solve the problems that a Schiff base type rare-earth metal complex is complex in synthetic method, is relatively low in yield, cannot realize batch production and can hardly emit white light. The white light material EuxDy1-xZn2L2(Hfac)6 has a crystal system of a monoclinic system and a space group of P21/c, and the value range of x is more than or equal to 0.03 and less than or equal to 0.05. The preparation method comprises: 1, preparing Zn2L2; 2, preparing a Zn2L2 trichloromethane solution; 3, preparing a mixed solution B; 4, preparing a preform; and 5, carrying out diffusion culture on n-hexane. The excitation wavelength of the white light material EuxDy1-xZn2L2(Hfac)6 is 300-320nm; and according to the preparation method disclosed by the invention, the white light material EuxDy1-xZn2L2(Hfac)6 can be obtained.
Description
Technical field
The present invention relates to white light emitting material and preparation method thereof.
Background technology
Rare earth luminescence absorbs energy by organic ligand, by intramolecular energy transfer, by transmission ofenergy to rare earth ion, and then sensitization rare earth luminescence.And part transferring energy is transmitted to rare earth ion by the excited singlet state of part or triplet state, wherein triplet state is in the majority.But organic ligand in order to can absorbing wavelength multidigit needed for effectively sensitization VISIBLE LIGHT EMISSION rare earth ion in ultraviolet region, and excitation energy is high, can damage organism, and makes organism self produce fluorescence, distrubed test data.This is not obviously suitable for the scientific research of organism.In order to reduce excitation wavelength needed for organic ligand, transition metal complex can be utilized for part, carry out coordination with rare earth ion, thus sensitization is rare earth luminous.Wherein transition metal is as sensitizing agent, by transmission ofenergy to rare earth ion or organic ligand, improves energy transfer efficiency, enhances molecular radiation transition, thus improve the luminescent properties of rare earth compound.
DeCola reported first in 2005 Ir (III)-Eu (III) bimetal complexes, this title complex adopts the carboxylic acid derivative of Phenyltriazole as bridge ligand, wherein (N^N) site and Ir (III) coordination, carboxyl site and rare earth Eu (III) coordination.Part energy can be transferred to Eu (III) by Ir (III) title complex, the white light that the ruddiness of the blue green light and Eu (III) title complex that finally obtain Ir (III) title complex mixes.The example that title complex emits white light is little, by literature search, generally carrys out the white light emission in practical function compound by three primary colours in unit molecule, or can produce white variable photoluminescence phenomenon during conversion excitation wavelength.Utilize sensitizing agent to pass through in the function rare earth compound of " antenna effect " sensitization rare earth transmitting, the rare earth that compound often presents remaining emission and the sensitization coming from sensitizing agent is launched.By regulating the emitting performance of sensitizing agent and controlling rate of energy transfer and efficiency, just can make full use of this " dual emission " spectral response curve and develop the advanced luminescent material with white light emission performance.Such as when adopt 400nm optical excitation shown in Ir
iII 2-Eu
iIIcompound, this compound will emit simultaneously come from Ir
iIIthe remaining green light emission band of building block and with Eu
iIIcentered by red emission band, these two kinds of emission bands just form complementary light, finally cause this compound to have white light emission performance.Eu
iIIcentered by the complementary color of red emission band be green light (λ ≈ 480nm), if by good green light emissive material and the ruddiness compound hydridization containing europium, just good white light emitting material can be obtained.Chen Zhong rather reports a few example and synthesizes 8-hydroxyquinoline aluminum-europium Al that is simple, with low cost, good luminescence property
3eu
2, zinc-europium Zn
2eu and zinc-samarium Zn
2sm
2heteronu clear metal complex, this type of title complex is all white light rare earth emissive material, and the synthesis step of this kind of hybrid compounds and cost are well below Ir
iII 2-Eu
iIIwhite light emitting material.8-hydroxyquinoline aluminum, Zn complex relatively easily synthesize, the hapto that the periphery of part is free, can continue and rare-earth ion coordination.By literature search, we find that current Zn-Ln Heteronu clear metal complex is mainly with the title complex that schiff bases is constructed, zinc presence of Schiff-base complex has the ability of good transmitting visible ray, the antenna group that the Huang Weiguo of Hong Kong Baptist University takes the lead in it can be used as sensitization rare earth ion near-infrared luminous synthesizes schiff bases Zn-Ln Heteronu clear metal complex, the people such as the Jones of Texas ,Usa university and the Lv Xingqiang of NORTHWEST CHINA university had synthesized a large amount of schiff bases double-core or multinuclear Zn-Ln Heteronu clear metal complex afterwards, think that energy donor in title complex derives from part usually by antenna effect spectrum and quantum chemical method
3lC or
1lC (the inner triplet state of part or singlet state charge transtion) excited state.
The general productive rate of Schiff bases rare earth metal complex is low, and the synthetic method of title complex is complicated, cannot produce in a large number.
Summary of the invention
The synthetic method that the object of the invention is to solve existing Schiff bases rare earth metal complex is complicated, and productive rate is lower, not can manufacture and is difficult to the problem emitted white light, and provide a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6and preparation method thereof.
A kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6crystallographic system be oblique system; Spacer is P21/c; Described Eu
xdy
1-xzn
2l
2(Hfac)
6the span of middle x is 0.03≤x≤0.05.
A kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method, complete according to the following steps:
One, Zn is prepared
2l
2;
1. 1,8-diamino-3,6-dioxaoctane methanol solution, is prepared: be dissolved in methyl alcohol by 1,8-diamino-3,6-dioxaoctane, obtain 1,8-diamino-3,6-dioxaoctane methanol solution;
Step one 1. described in the amount of substance of 1,8-diamino-3,6-dioxaoctane and the volume ratio of methyl alcohol be (8mmol ~ 12mmol): 10mL;
2., by salicylic aldehyde be dissolved in methyl alcohol, obtain salicylic aldehyde methanol solution;
Step one 2. described in the amount of substance of salicylic aldehyde and the volume ratio of methyl alcohol be (15mmol ~ 25mmol): 20mL;
3., by 1,8-diamino-3,6-dioxaoctane methanol solution salicylic aldehyde methanol solution is added dropwise to the rate of addition of 10/min ~ 15 droplet/min, then the 5h that refluxes at temperature is 65 DEG C, then be cooled to room temperature, obtain yellow clear solution; Again yellow clear solution is left standstill 10h ~ 12h at-5 DEG C, then filter, obtain H
2l, H
2l is 1,8-diamino-3,6-dioxaoctane salicylaldehyde;
Step one 3. described in 1,8-diamino-3,6-dioxaoctane methanol solution and the volume ratio of salicylic aldehyde methanol solution be 1:2;
4., by Zn (OAc)
22H
2o is dissolved in distilled water, obtains Zn (OAc)
2the aqueous solution;
Step one 4. described in Zn (OAc)
22H
2the amount of substance of O and the volume ratio of distilled water are (25mmol ~ 30mmol): 25mL;
5. the H, 3. step obtained
2l is dissolved in dehydrated alcohol, obtains H
2l ethanol solution;
Step one 5. described in H
2the amount of substance of L and the volume ratio of dehydrated alcohol are (25mmol ~ 30mmol): 25mL;
6., by Zn (OAc)
2the aqueous solution and H
2l ethanol solution mixes, and obtains mixed solution A; Reflux mixed solution A at temperature is 60 DEG C 2h ~ 3h again, naturally cool to room temperature again, stirring reaction 5h ~ 6h under room temperature and stirring velocity are 70r/min ~ 80r/min again, then filter, obtain yellow mercury oxide material, first distilled water is used to clean 3 times ~ 5 times to yellow mercury oxide material, re-use massfraction be 20% ~ 30% sodium hydrogen carbonate solution clean 3 times ~ 5 times, finally use washes of absolute alcohol 3 times ~ 5 times, more at room temperature dry 24h, grind again, obtain Zn
2l
2, be 1,8-diamino-3,6-dioxaoctane salicylaldehyde Zn complex;
Step one 6. described in mixed solution A in Zn (OAc)
2with H
2the mol ratio of L is 1:1;
Two, the Zn 6. step one obtained
2l
2be dissolved in trichloromethane, obtain Zn
2l
2chloroform soln;
Zn described in step 2
2l
2zn in chloroform soln
2l
2volumetric molar concentration be 0.1mol/L;
Three, hexafluoroacetylacetone rare-earth salts is dissolved in trichloromethane, then adds Zn in trichloromethane
2l
2chloroform soln, obtains mixing solutions B;
Hexafluoroacetylacetone rare-earth salts and Zn in mixing solutions B described in step 3
2l
2amount of substance than for 1:1;
Hexafluoroacetylacetone rare-earth salts described in step 3 is Eu (Hfac)
3with Dy (Hfac)
3mixture; Eu (Hfac) in described hexafluoroacetylacetone rare-earth salts
3with Dy (Hfac)
3amount of substance than for x:(1-x), wherein the span of x is 0.03≤x≤0.05;
The amount of substance of the hexafluoroacetylacetone rare-earth salts described in step 3 and the volume ratio (0.02mol ~ 0.03mol) of trichloromethane: 1L;
Four, the mixing solutions B obtained in step 3 is kept 1h ~ 1.5h at temperature is 88 DEG C ~ 92 DEG C, obtain precast body;
Five, the precast body self-heating obtained in step 4 is cooled to room temperature, then puts in container, then drip normal hexane with the rate of addition of 10/min ~ 15 droplet/min in container, again container is sealed, at room temperature keep 10 days ~ 15 days again, obtain yellow crystals, be white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6, complete white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method;
The volume ratio of the normal hexane described in step 5 and precast body is (2 ~ 4): 1.
Eu of the present invention (Hfac)
3for hexafluoroacetylacetone europium; Described Dy (Hfac)
3for hexafluoroacetylacetone dysprosium;
White light emitting material Eu of the present invention
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 330nm, can obtain controlled CIE white light coordinates after exciting, described CIE coordinate is positioned at: x=0.341, y=0.342;
White light emitting material Eu of the present invention
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm; White light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.
Principle of the present invention:
Because the radius of rare earth ion europium and dysprosium is too close, crystallography cannot be distinguished, therefore Eu
xdy
1-xzn
2l
2(Hfac)
6crystal data exact solution can not separate out the ratio of europium and dysprosium.
Advantage of the present invention:
One, the white light emitting material Eu for preparing of the present invention
xdy
1-xzn
2l
2(Hfac)
6productive rate high, reach more than 45.8%;
Two, the white light emitting material Eu for preparing of the present invention
xdy
1-xzn
2l
2(Hfac)
6synthetic method simple, repeatability is strong;
Three, the white light emitting material Eu for preparing of the present invention
xdy
1-xzn
2l
2(Hfac)
6for the white light emitting material of single-component, multi-wave length illuminating, can be applicable to the application of white light emitting material, avoid the operations such as multi-component proportioning;
Four, the white light emitting material Eu for preparing of the present invention
xdy
1-xzn
2l
2(Hfac)
6quality white light controlled fine setting in building-up process;
Five, white light emitting material Eu of the present invention
xdy
1-xzn
2l
2(Hfac)
6product can synthesize in atmosphere, require simple to plant and instrument, with low cost, synthesis cycle is short, can be applicable to the application of white light emitting material.
The present invention can obtain a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6.
Accompanying drawing explanation
Fig. 1 is Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6the schematic arrangement of crystal;
Fig. 2 is Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6the two dimensional structure schematic diagram of crystal;
Fig. 3 is infrared spectrum, and wherein curve 1 is the Zn that 6. embodiment one step one is prepared
2l
2infrared curve, a kind of white light emitting material Eu that curve 2 is prepared for embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6infrared curve;
Fig. 4 is white light emitting material Eu prepared by embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6fluorescence spectrum figure under 310nm wavelength;
Fig. 5 is white light emitting material Eu prepared by embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6cIE coordinate diagram;
Fig. 6 is XRD spectra, and wherein curve 1 is Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6xRD curve, curve 2 be simultaneous test two prepare Dy
2zn
2l
2(Hfac)
6xRD curve, a kind of white light emitting material Eu that curve 3 is prepared for embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6xRD curve.
Embodiment
Embodiment one: present embodiment is a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6crystallographic system be oblique system; Spacer is P21/c; Described Eu
xdy
1-xzn
2l
2(Hfac)
6the span of middle x is 0.03≤x≤0.05.
Embodiment two: the difference of present embodiment and embodiment one is: described white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm.Other are identical with embodiment one.
Embodiment three: the difference of one of present embodiment and embodiment one or two is: described white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.Other are identical with embodiment one or two.
Embodiment four: present embodiment is a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method complete according to the following steps:
One, Zn is prepared
2l
2;
1. 1,8-diamino-3,6-dioxaoctane methanol solution, is prepared: be dissolved in methyl alcohol by 1,8-diamino-3,6-dioxaoctane, obtain 1,8-diamino-3,6-dioxaoctane methanol solution;
Step one 1. described in the amount of substance of 1,8-diamino-3,6-dioxaoctane and the volume ratio of methyl alcohol be (8mmol ~ 12mmol): 10mL;
2., by salicylic aldehyde be dissolved in methyl alcohol, obtain salicylic aldehyde methanol solution;
Step one 2. described in the amount of substance of salicylic aldehyde and the volume ratio of methyl alcohol be (15mmol ~ 25mmol): 20mL;
3., by 1,8-diamino-3,6-dioxaoctane methanol solution salicylic aldehyde methanol solution is added dropwise to the rate of addition of 10/min ~ 15 droplet/min, then the 5h that refluxes at temperature is 65 DEG C, then be cooled to room temperature, obtain yellow clear solution; Again yellow clear solution is left standstill 10h ~ 12h at-5 DEG C, then filter, obtain H
2l, H
2l is 1,8-diamino-3,6-dioxaoctane salicylaldehyde;
Step one 3. described in 1,8-diamino-3,6-dioxaoctane methanol solution and the volume ratio of salicylic aldehyde methanol solution be 1:2;
4., by Zn (OAc)
22H
2o is dissolved in distilled water, obtains Zn (OAc)
2the aqueous solution;
Step one 4. described in Zn (OAc)
22H
2the amount of substance of O and the volume ratio of distilled water are (25mmol ~ 30mmol): 25mL;
5. the H, 3. step obtained
2l is dissolved in dehydrated alcohol, obtains H
2l ethanol solution;
Step one 5. described in H
2the amount of substance of L and the volume ratio of dehydrated alcohol are (25mmol ~ 30mmol): 25mL;
6., by Zn (OAc)
2the aqueous solution and H
2l ethanol solution mixes, and obtains mixed solution A; Reflux mixed solution A at temperature is 60 DEG C 2h ~ 3h again, naturally cool to room temperature again, stirring reaction 5h ~ 6h under room temperature and stirring velocity are 70r/min ~ 80r/min again, then filter, obtain yellow mercury oxide material, first distilled water is used to clean 3 times ~ 5 times to yellow mercury oxide material, re-use massfraction be 20% ~ 30% sodium hydrogen carbonate solution clean 3 times ~ 5 times, finally use washes of absolute alcohol 3 times ~ 5 times, more at room temperature dry 24h, grind again, obtain Zn
2l
2, be 1,8-diamino-3,6-dioxaoctane salicylaldehyde Zn complex;
Step one 6. described in mixed solution A in Zn (OAc)
2with H
2the mol ratio of L is 1:1;
Two, the Zn 6. step one obtained
2l
2be dissolved in trichloromethane, obtain Zn
2l
2chloroform soln;
Zn described in step 2
2l
2zn in chloroform soln
2l
2volumetric molar concentration be 0.1mol/L;
Three, hexafluoroacetylacetone rare-earth salts is dissolved in trichloromethane, then adds Zn in trichloromethane
2l
2chloroform soln, obtains mixing solutions B;
Hexafluoroacetylacetone rare-earth salts and Zn in mixing solutions B described in step 3
2l
2amount of substance than for 1:1;
Hexafluoroacetylacetone rare-earth salts described in step 3 is Eu (Hfac)
3with Dy (Hfac)
3mixture; Eu (Hfac) in described hexafluoroacetylacetone rare-earth salts
3with Dy (Hfac)
3amount of substance than for x:(1-x), wherein the span of x is 0.03≤x≤0.05;
The amount of substance of the hexafluoroacetylacetone rare-earth salts described in step 3 and the volume ratio (0.02mol ~ 0.03mol) of trichloromethane: 1L;
Four, the mixing solutions B obtained in step 3 is kept 1h ~ 1.5h at temperature is 88 DEG C ~ 92 DEG C, obtain precast body;
Five, the precast body self-heating obtained in step 4 is cooled to room temperature, then puts in container, then drip normal hexane with the rate of addition of 10/min ~ 15 droplet/min in container, again container is sealed, at room temperature keep 10 days ~ 15 days again, obtain yellow crystals, be white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6, complete white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method;
The volume ratio of the normal hexane described in step 5 and precast body is (2 ~ 4): 1.
Eu (Hfac) described in present embodiment
3for hexafluoroacetylacetone europium; Described Dy (Hfac)
3for hexafluoroacetylacetone dysprosium;
White light emitting material Eu described in present embodiment
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 330nm, can obtain controlled CIE white light coordinates after exciting, described CIE coordinate is positioned at: x=0.341, y=0.342;
White light emitting material Eu described in present embodiment
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm; White light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.
The principle of present embodiment:
Because the radius of rare earth ion europium and dysprosium is too close, crystallography cannot be distinguished, therefore Eu
xdy
1-xzn
2l
2(Hfac)
6crystal data exact solution can not separate out the ratio of europium and dysprosium.
The advantage of present embodiment:
One, the white light emitting material Eu for preparing of present embodiment
xdy
1-xzn
2l
2(Hfac)
6productive rate high, reach more than 45.8%;
Two, the white light emitting material Eu for preparing of present embodiment
xdy
1-xzn
2l
2(Hfac)
6synthetic method simple, repeatability is strong;
Three, the white light emitting material Eu for preparing of present embodiment
xdy
1-xzn
2l
2(Hfac)
6for the white light emitting material of single-component, multi-wave length illuminating, can be applicable to the application of white light emitting material, avoid the operations such as multi-component proportioning;
Four, the white light emitting material Eu for preparing of present embodiment
xdy
1-xzn
2l
2(Hfac)
6quality white light controlled fine setting in building-up process;
Five, the white light emitting material Eu of present embodiment
xdy
1-xzn
2l
2(Hfac)
6product can synthesize in atmosphere, require simple to plant and instrument, with low cost, synthesis cycle is short, can be applicable to the application of white light emitting material.
Present embodiment can obtain a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6.
Embodiment five: the difference of present embodiment and embodiment four is: in step 4, the mixing solutions B obtained in step 3 is kept 1h at temperature is 90 DEG C, obtain precast body.Other are identical with embodiment four.
Embodiment six: the difference of one of present embodiment and embodiment four or five is: the hexafluoroacetylacetone rare-earth salts described in step 3 is Eu (Hfac)
3with Dy (Hfac)
3mixture; Eu (Hfac) in described hexafluoroacetylacetone rare-earth salts
3with Dy (Hfac)
3amount of substance than for x:(1-x), wherein the span of x is x=0.042.Other are identical with embodiment four or five.
Embodiment seven: the difference of one of present embodiment and embodiment four to six is: in step 5, the precast body self-heating obtained in step 4 is cooled to room temperature, put into again in container, normal hexane is dripped with the rate of addition of 13/min again in container, again container is sealed, at room temperature keep 13 days again, obtain yellow crystals, be white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6, complete white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method; The volume ratio of the normal hexane described in step 5 and precast body is 3:1.Other are identical with embodiment four to six.
Embodiment eight: the difference of one of present embodiment and embodiment four to seven is: the white light emitting material Eu described in step 5
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm.Other are identical with embodiment four to seven.
Embodiment nine: the difference of one of present embodiment and embodiment four to eight is: the white light emitting material Eu described in step 5
xdy
1-xzn
2l
2(Hfac)
6wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.Other are identical with embodiment four to eight.
Embodiment ten: the difference of one of present embodiment and embodiment four to nine is: the white light emitting material Eu described in step 5
xdy
1-xzn
2l
2(Hfac)
6crystallographic system be oblique system; Spacer is P21/c; Described Eu
xdy
1-xzn
2l
2(Hfac)
6the span of middle x is 0.03≤x≤0.05.Other are identical with embodiment four to nine.
Embodiment one: a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method complete according to the following steps:
One, Zn is prepared
2l
2;
1. 1,8-diamino-3,6-dioxaoctane methanol solution, is prepared: be dissolved in methyl alcohol by 1,8-diamino-3,6-dioxaoctane, obtain 1,8-diamino-3,6-dioxaoctane methanol solution;
Step one 1. described in the amount of substance of 1,8-diamino-3,6-dioxaoctane and the volume ratio of methyl alcohol be 10mmol:10mL;
2., by salicylic aldehyde be dissolved in methyl alcohol, obtain salicylic aldehyde methanol solution;
Step one 2. described in the amount of substance of salicylic aldehyde and the volume ratio of methyl alcohol be 20mmol:20mL;
3., by 1,8-diamino-3,6-dioxaoctane methanol solution salicylic aldehyde methanol solution is added dropwise to the rate of addition of 13/min, then the 5h that refluxes at temperature is 65 DEG C, then be cooled to room temperature, obtain yellow clear solution; Again yellow clear solution is left standstill 12h at-5 DEG C, then filter, obtain H
2l, H
2l is 1,8-diamino-3,6-dioxaoctane salicylaldehyde;
Step one 3. described in 1,8-diamino-3,6-dioxaoctane methanol solution and the volume ratio of salicylic aldehyde methanol solution be 1:2;
4., by Zn (OAc)
22H
2o is dissolved in distilled water, obtains Zn (OAc)
2the aqueous solution;
Step one 4. described in Zn (OAc)
22H
2the amount of substance of O and the volume ratio of distilled water are 25mmol:25mL;
5. the H, 3. step obtained
2l is dissolved in dehydrated alcohol, obtains H
2l ethanol solution;
Step one 5. described in H
2the amount of substance of L and the volume ratio of dehydrated alcohol are 25mmol:25mL;
6., by Zn (OAc)
2the aqueous solution and H
2l ethanol solution mixes, and obtains mixed solution A; Reflux mixed solution A at temperature is 60 DEG C 3h again, naturally cool to room temperature again, be at room temperature stirring reaction 5.5h under 80r/min with stirring velocity again, then filter, obtain yellow mercury oxide material, first distilled water is used to clean 4 times to yellow mercury oxide material, re-use massfraction be 25% sodium hydrogen carbonate solution clean 4 times, finally use washes of absolute alcohol 4 times, more at room temperature dry 24h, grind again, obtain Zn
2l
2, be 1,8-diamino-3,6-dioxaoctane salicylaldehyde Zn complex;
Step one 6. described in mixed solution A in Zn (OAc)
2with H
2the mol ratio of L is 1:1;
Two, the Zn 6. step one obtained
2l
2be dissolved in trichloromethane, obtain Zn
2l
2chloroform soln;
Zn described in step 2
2l
2zn in chloroform soln
2l
2volumetric molar concentration be 0.1mol/L;
Three, hexafluoroacetylacetone rare-earth salts is dissolved in trichloromethane, then adds Zn in trichloromethane
2l
2chloroform soln, obtains mixing solutions B;
Hexafluoroacetylacetone rare-earth salts and Zn in mixing solutions B described in step 3
2l
2amount of substance than for 1:1;
Hexafluoroacetylacetone rare-earth salts described in step 3 is Eu (Hfac)
3with Dy (Hfac)
3mixture; Eu (Hfac) in described hexafluoroacetylacetone rare-earth salts
3with Dy (Hfac)
3amount of substance than for x:(1-x), wherein the span of x is x=0.042;
The amount of substance of hexafluoroacetylacetone rare-earth salts described in step 3 and the volume ratio 0.02mol:1L of trichloromethane;
Four, the mixing solutions B obtained in step 3 is kept 1h at temperature is 90 DEG C, obtain precast body;
Five, the precast body self-heating obtained in step 4 is cooled to room temperature, then puts in container, then drip normal hexane with the rate of addition of 13/min in container, again container is sealed, at room temperature keep 13 days again, obtain yellow crystals, be white light emitting material Eu
0.042dy
0.958zn
2l
2(Hfac)
6, complete white light emitting material Eu
0.042dy
0.958zn
2l
2(Hfac)
6preparation method; The volume ratio of the normal hexane described in step 5 and precast body is 3:1.
White light emitting material Eu prepared by embodiment one
0.042dy
0.958zn
2l
2(Hfac)
6productive rate be 43.8%.
Simultaneous test one: a kind of Eu
2zn
2l
2(Hfac)
6the preparation method of crystal, completes according to the following steps:
One, Zn is prepared
2l
2;
1. 1,8-diamino-3,6-dioxaoctane methanol solution, is prepared: be dissolved in methyl alcohol by 1,8-diamino-3,6-dioxaoctane, obtain 1,8-diamino-3,6-dioxaoctane methanol solution;
Step one 1. described in the amount of substance of 1,8-diamino-3,6-dioxaoctane and the volume ratio of methyl alcohol be 10mmol:10mL;
2., by salicylic aldehyde be dissolved in methyl alcohol, obtain salicylic aldehyde methanol solution;
Step one 2. described in the amount of substance of salicylic aldehyde and the volume ratio of methyl alcohol be 20mmol:20mL;
3., by 1,8-diamino-3,6-dioxaoctane methanol solution salicylic aldehyde methanol solution is added dropwise to the rate of addition of 13/min, then the 5h that refluxes at temperature is 65 DEG C, then be cooled to room temperature, obtain yellow clear solution; Again yellow clear solution is left standstill 12h at-5 DEG C, then filter, obtain H
2l, H
2l is 1,8-diamino-3,6-dioxaoctane salicylaldehyde;
Step one 3. described in 1,8-diamino-3,6-dioxaoctane methanol solution and the volume ratio of salicylic aldehyde methanol solution be 1:2;
4., by Zn (OAc)
22H
2o is dissolved in distilled water, obtains Zn (OAc)
2the aqueous solution;
Step one 4. described in Zn (OAc)
22H
2the amount of substance of O and the volume ratio of distilled water are 25mmol:25mL;
5. the H, 3. step obtained
2l is dissolved in dehydrated alcohol, obtains H
2l ethanol solution;
Step one 5. described in H
2the amount of substance of L and the volume ratio of dehydrated alcohol are 25mmol:25mL;
6., by Zn (OAc)
2the aqueous solution and H
2l ethanol solution mixes, and obtains mixed solution A; Reflux mixed solution A at temperature is 60 DEG C 3h again, naturally cool to room temperature again, be at room temperature stirring reaction 5.5h under 80r/min with stirring velocity again, then filter, obtain yellow mercury oxide material, first distilled water is used to clean 4 times to yellow mercury oxide material, re-use massfraction be 25% sodium hydrogen carbonate solution clean 4 times, finally use washes of absolute alcohol 4 times, more at room temperature dry 24h, grind again, obtain Zn
2l
2, be 1,8-diamino-3,6-dioxaoctane salicylaldehyde Zn complex;
Step one 6. described in mixed solution A in Zn (OAc)
2with H
2the mol ratio of L is 1:1;
Two, the Zn 6. step one obtained
2l
2be dissolved in trichloromethane, obtain Zn
2l
2chloroform soln;
Zn described in step 2
2l
2zn in chloroform soln
2l
2volumetric molar concentration be 0.1mol/L;
Three, by Eu (Hfac)
3be dissolved in trichloromethane, then add Zn in trichloromethane
2l
2chloroform soln, obtains mixing solutions B;
Eu (Hfac) in mixing solutions B described in step 3
3with Zn
2l
2amount of substance than for 1:1;
Eu (Hfac) described in step 3
3amount of substance and the volume ratio 0.02mol:1L of trichloromethane;
Four, the mixing solutions B obtained in step 3 is kept 1h at temperature is 90 DEG C, obtain precast body;
Five, the precast body self-heating obtained in step 4 is cooled to room temperature, then puts in container, then drip normal hexane with the rate of addition of 13/min in container, then container is sealed, more at room temperature keep 13 days, obtain Eu
2zn
2l
2(Hfac)
6crystal, completes Eu
2zn
2l
2(Hfac)
6the preparation method of crystal; The volume ratio of the normal hexane described in step 5 and precast body is 3:1.
Simultaneous test two: a kind of Dy
2zn
2l
2(Hfac)
6the preparation method of crystal, completes according to the following steps:
One, Zn is prepared
2l
2;
1. 1,8-diamino-3,6-dioxaoctane methanol solution, is prepared: be dissolved in methyl alcohol by 1,8-diamino-3,6-dioxaoctane, obtain 1,8-diamino-3,6-dioxaoctane methanol solution;
Step one 1. described in the amount of substance of 1,8-diamino-3,6-dioxaoctane and the volume ratio of methyl alcohol be 10mmol:10mL;
2., by salicylic aldehyde be dissolved in methyl alcohol, obtain salicylic aldehyde methanol solution;
Step one 2. described in the amount of substance of salicylic aldehyde and the volume ratio of methyl alcohol be 20mmol:20mL;
3., by 1,8-diamino-3,6-dioxaoctane methanol solution salicylic aldehyde methanol solution is added dropwise to the rate of addition of 13/min, then the 5h that refluxes at temperature is 65 DEG C, then be cooled to room temperature, obtain yellow clear solution; Again yellow clear solution is left standstill 12h at-5 DEG C, then filter, obtain H
2l, H
2l is 1,8-diamino-3,6-dioxaoctane salicylaldehyde;
Step one 3. described in 1,8-diamino-3,6-dioxaoctane methanol solution and the volume ratio of salicylic aldehyde methanol solution be 1:2;
4., by Zn (OAc)
22H
2o is dissolved in distilled water, obtains Zn (OAc)
2the aqueous solution;
Step one 4. described in Zn (OAc)
22H
2the amount of substance of O and the volume ratio of distilled water are 25mmol:25mL;
5. the H, 3. step obtained
2l is dissolved in dehydrated alcohol, obtains H
2l ethanol solution;
Step one 5. described in H
2the amount of substance of L and the volume ratio of dehydrated alcohol are 25mmol:25mL;
6., by Zn (OAc)
2the aqueous solution and H
2l ethanol solution mixes, and obtains mixed solution A; Reflux mixed solution A at temperature is 60 DEG C 3h again, naturally cool to room temperature again, be at room temperature stirring reaction 5.5h under 80r/min with stirring velocity again, then filter, obtain yellow mercury oxide material, first distilled water is used to clean 4 times to yellow mercury oxide material, re-use massfraction be 25% sodium hydrogen carbonate solution clean 4 times, finally use washes of absolute alcohol 4 times, more at room temperature dry 24h, grind again, obtain Zn
2l
2, be 1,8-diamino-3,6-dioxaoctane salicylaldehyde Zn complex;
Step one 6. described in mixed solution A in Zn (OAc)
2with H
2the mol ratio of L is 1:1;
Two, the Zn 6. step one obtained
2l
2be dissolved in trichloromethane, obtain Zn
2l
2chloroform soln;
Zn described in step 2
2l
2zn in chloroform soln
2l
2volumetric molar concentration be 0.1mol/L;
Three, by Dy (Hfac)
3be dissolved in trichloromethane, then add Zn in trichloromethane
2l
2chloroform soln, obtains mixing solutions B;
Dy (Hfac) in mixing solutions B described in step 3
3with Zn
2l
2amount of substance than for 1:1;
Dy (Hfac) described in step 3
3amount of substance and the volume ratio 0.02mol:1L of trichloromethane;
Four, the mixing solutions B obtained in step 3 is kept 1h at temperature is 90 DEG C, obtain precast body;
Five, the precast body self-heating obtained in step 4 is cooled to room temperature, then puts in container, then drip normal hexane with the rate of addition of 13/min in container, then container is sealed, more at room temperature keep 13 days, obtain Dy
2zn
2l
2(Hfac)
6crystal, completes Dy
2zn
2l
2(Hfac)
6the preparation method of crystal; The volume ratio of the normal hexane described in step 5 and precast body is 3:1.
Utilize the Eu that RigakuRaxis-RapidX-x ray diffractometer x is prepared simultaneous test one
2zn
2l
2(Hfac)
6with Dy prepared by simultaneous test two
2zn
2l
2(Hfac)
6crystalline structure measures, and structure is identical, and test data lists in table 1, and table 1 is Eu
2zn
2l
2(Hfac)
6and Zn
2l
2dy
2(hfac)
6crystalline structure refine data:
Table 1
Fig. 1 is Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6the schematic arrangement of crystal;
Fig. 2 is Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6the two dimensional structure schematic diagram of crystal;
From Fig. 1 and Fig. 2, Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6four central atoms of crystal are in same plane.
Fig. 3 is infrared spectrum, and wherein curve 1 is the Zn that 6. embodiment one step one is prepared
2l
2infrared curve, a kind of white light emitting material Eu that curve 2 is prepared for embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6infrared curve;
As can be seen from Figure 3, a kind of white light emitting material Eu of preparing of embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6the infrared absorption of functional group.
Fig. 4 is white light emitting material Eu prepared by embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6fluorescence spectrum figure under 310nm wavelength;
As can be seen from Figure 4, the white light emitting material Eu for preparing of embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6from blue light region to green Region and red light district.
Fig. 5 is white light emitting material Eu prepared by embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6cIE coordinate diagram;
As can be seen from Figure 5, the white light emitting material Eu for preparing of embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6in white light area, close to pure white light coordinate (0.333,0.333)
Fig. 6 is XRD spectra, and wherein curve 1 is Eu prepared by simultaneous test one
2zn
2l
2(Hfac)
6xRD curve, curve 2 be simultaneous test two prepare Dy
2zn
2l
2(Hfac)
6xRD curve, a kind of white light emitting material Eu that curve 3 is prepared for embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6xRD curve.
As can be seen from Figure 6, a kind of white light emitting material Eu of preparing of embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6identical with the structure of dysprosium title complex with europium.
Eu (Hfac) described in simultaneous test one
3for hexafluoroacetylacetone europium; Dy (Hfac) described in simultaneous test two
3for hexafluoroacetylacetone dysprosium;
White light emitting material Eu prepared by embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 330nm, can obtain controlled CIE white light coordinates after exciting, described CIE coordinate is positioned at: x=0.341, y=0.342;
A kind of white light emitting material Eu prepared by embodiment one step 5
0.042dy
0.958zn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm; Wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.
White light emitting material Eu prepared by embodiment one
0.042dy
0.958zn
2l
2(Hfac)
6productive rate high, reach 68%.
Claims (10)
1. a white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6, it is characterized in that a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6crystallographic system be oblique system; Spacer is P21/c; Described Eu
xdy
1-xzn
2l
2(Hfac)
6the span of middle x is 0.03≤x≤0.05.
2. a kind of white light emitting material Eu according to claim 1
xdy
1-xzn
2l
2(Hfac)
6, it is characterized in that described white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm.
3. a kind of white light emitting material Eu according to claim 1
xdy
1-xzn
2l
2(Hfac)
6, it is characterized in that described white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.
4. a white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that a kind of white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method complete according to the following steps:
One, Zn is prepared
2l
2;
1. 1,8-diamino-3,6-dioxaoctane methanol solution, is prepared: be dissolved in methyl alcohol by 1,8-diamino-3,6-dioxaoctane, obtain 1,8-diamino-3,6-dioxaoctane methanol solution;
Step one 1. described in the amount of substance of 1,8-diamino-3,6-dioxaoctane and the volume ratio of methyl alcohol be (8mmol ~ 12mmol): 10mL;
2., by salicylic aldehyde be dissolved in methyl alcohol, obtain salicylic aldehyde methanol solution;
Step one 2. described in the amount of substance of salicylic aldehyde and the volume ratio of methyl alcohol be (15mmol ~ 25mmol): 20mL;
3., by 1,8-diamino-3,6-dioxaoctane methanol solution salicylic aldehyde methanol solution is added dropwise to the rate of addition of 10/min ~ 15 droplet/min, then the 5h that refluxes at temperature is 65 DEG C, then be cooled to room temperature, obtain yellow clear solution; Again yellow clear solution is left standstill 10h ~ 12h at-5 DEG C, then filter, obtain H
2l, H
2l is 1,8-diamino-3,6-dioxaoctane salicylaldehyde;
Step one 3. described in 1,8-diamino-3,6-dioxaoctane methanol solution and the volume ratio of salicylic aldehyde methanol solution be 1:2;
4., by Zn (OAc)
22H
2o is dissolved in distilled water, obtains Zn (OAc)
2the aqueous solution;
Step one 4. described in Zn (OAc)
22H
2the amount of substance of O and the volume ratio of distilled water are (25mmol ~ 30mmol): 25mL;
5. the H, 3. step obtained
2l is dissolved in dehydrated alcohol, obtains H
2l ethanol solution;
Step one 5. described in H
2the amount of substance of L and the volume ratio of dehydrated alcohol are (25mmol ~ 30mmol): 25mL;
6., by Zn (OAc)
2the aqueous solution and H
2l ethanol solution mixes, and obtains mixed solution A; Reflux mixed solution A at temperature is 60 DEG C 2h ~ 3h again, naturally cool to room temperature again, stirring reaction 5h ~ 6h under room temperature and stirring velocity are 70r/min ~ 80r/min again, then filter, obtain yellow mercury oxide material, first distilled water is used to clean 3 times ~ 5 times to yellow mercury oxide material, re-use massfraction be 20% ~ 30% sodium hydrogen carbonate solution clean 3 times ~ 5 times, finally use washes of absolute alcohol 3 times ~ 5 times, more at room temperature dry 24h, grind again, obtain Zn
2l
2, be 1,8-diamino-3,6-dioxaoctane salicylaldehyde Zn complex;
Step one 6. described in mixed solution A in Zn (OAc)
2with H
2the mol ratio of L is 1:1;
Two, the Zn 6. step one obtained
2l
2be dissolved in trichloromethane, obtain Zn
2l
2chloroform soln;
Zn described in step 2
2l
2zn in chloroform soln
2l
2volumetric molar concentration be 0.1mol/L;
Three, hexafluoroacetylacetone rare-earth salts is dissolved in trichloromethane, then adds Zn in trichloromethane
2l
2chloroform soln, obtains mixing solutions B;
Hexafluoroacetylacetone rare-earth salts and Zn in mixing solutions B described in step 3
2l
2amount of substance than for 1:1;
Hexafluoroacetylacetone rare-earth salts described in step 3 is Eu (Hfac)
3with Dy (Hfac)
3mixture; Eu (Hfac) in described hexafluoroacetylacetone rare-earth salts
3with Dy (Hfac)
3amount of substance than for x:(1-x), wherein the span of x is 0.03≤x≤0.05;
The amount of substance of the hexafluoroacetylacetone rare-earth salts described in step 3 and the volume ratio (0.02mol ~ 0.03mol) of trichloromethane: 1L;
Four, the mixing solutions B obtained in step 3 is kept 1h ~ 1.5h at temperature is 88 DEG C ~ 92 DEG C, obtain precast body;
Five, the precast body self-heating obtained in step 4 is cooled to room temperature, then puts in container, then drip normal hexane with the rate of addition of 10/min ~ 15 droplet/min in container, again container is sealed, at room temperature keep 10 days ~ 15 days again, obtain yellow crystals, be white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6, complete white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method;
The volume ratio of the normal hexane described in step 5 and precast body is (2 ~ 4): 1.
5. a kind of white light emitting material Eu according to claim 4
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that, in step 4, the mixing solutions B obtained in step 3 is kept 1h at temperature is 90 DEG C, obtain precast body.
6. a kind of white light emitting material Eu according to claim 4
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that the hexafluoroacetylacetone rare-earth salts described in step 3 is Eu (Hfac)
3with Dy (Hfac)
3mixture; Eu (Hfac) in described hexafluoroacetylacetone rare-earth salts
3with Dy (Hfac)
3amount of substance than for x:(1-x), wherein the span of x is x=0.042.
7. a kind of white light emitting material Eu according to claim 4
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that, in step 5, the precast body self-heating obtained in step 4 is cooled to room temperature, put into again in container, normal hexane is dripped with the rate of addition of 13/min again in container, again container is sealed, at room temperature keep 13 days again, obtain yellow crystals, be white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6, complete white light emitting material Eu
xdy
1-xzn
2l
2(Hfac)
6preparation method; The volume ratio of the normal hexane described in step 5 and precast body is 3:1.
8. a kind of white light emitting material Eu according to claim 4
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that the white light emitting material Eu described in step 5
xdy
1-xzn
2l
2(Hfac)
6excitation wavelength be 300nm ~ 320nm.
9. a kind of white light emitting material Eu according to claim 4
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that the white light emitting material Eu described in step 5
xdy
1-xzn
2l
2(Hfac)
6wavelengths of white light after exciting is 400nm ~ 700nm, comprising 483nm blue light, 514nm green glow and 613nm ruddiness.
10. a kind of white light emitting material Eu according to claim 4
xdy
1-xzn
2l
2(Hfac)
6preparation method, it is characterized in that the white light emitting material Eu described in step 5
xdy
1-xzn
2l
2(Hfac)
6crystallographic system be oblique system; Spacer is P21/c; Described Eu
xdy
1-xzn
2l
2(Hfac)
6the span of middle x is 0.03≤x≤0.05.
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| CN106866983A (en) * | 2016-12-19 | 2017-06-20 | 江苏师范大学 | The regulation and control synthesis of low temperature white light rare earth organic coordination polymer and fluorescence regulation and control |
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| CN101812083A (en) * | 2009-07-16 | 2010-08-25 | 黑龙江大学 | Salicylaldehyde diamine rear earth coordination compound and synthesis method and application thereof |
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| CN101812083A (en) * | 2009-07-16 | 2010-08-25 | 黑龙江大学 | Salicylaldehyde diamine rear earth coordination compound and synthesis method and application thereof |
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| 贾蕊: "席夫碱3d-4f和4f-4f金属配合物的合成及荧光性质研究", 《黑龙江大学硕士学位论文》 * |
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|---|---|---|---|---|
| CN106866983A (en) * | 2016-12-19 | 2017-06-20 | 江苏师范大学 | The regulation and control synthesis of low temperature white light rare earth organic coordination polymer and fluorescence regulation and control |
| CN106866983B (en) * | 2016-12-19 | 2020-02-07 | 江苏师范大学 | Regulation synthesis and fluorescence regulation of low-temperature white light rare earth-organic coordination polymer |
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Application publication date: 20160330 |