CN106633089A - White-light luminescent material doped with rare earth coordination polymer and preparation method thereof - Google Patents
White-light luminescent material doped with rare earth coordination polymer and preparation method thereof Download PDFInfo
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Abstract
The invention provides a white-light luminescent material doped with Tb<3+>/Eu<3+> rare earth coordination polymer and a preparation method thereof, and belongs to the technical field of the luminescence and display. The white-light luminescent material is synthesized by using 2,5-dyhydroxy terephthalic acid as an organic-ligand, using a simple solvent thermal synthesis method, and doping two different proportions of the rear earth metal ions. A coordination compound prepared by the method can produce the feature red light emission of the ion Eu<3+> and the blue light emission of the ligand in the room temperature under the excitation of 370 nm of the ultraviolet, and the relative strength of the red light emission and the blue light emission can be adjusted by adjusting the content of the ion Eu<3+> in the coordination compound, so that the white light emission of the coordination compound can be realized. The preparation method is simple, and the raw materials can be easily obtained. The white-light luminescent material doped with Tb<3+>/Eu<3+> rare earth coordination polymer can be used as a novel white-light luminescent material.
Description
Technical field
The invention belongs to luminous and display technology field, and in particular to a kind of white light emitting material, molecular formula is
{[Tb0.695Eu0.305(DHBDC)3(DMF)4](DMF)2}nCoordination compound preparation method.
Background technology
White light emitting diode（WLED）Due to many advantages such as luminous efficiency height, the low, long service life of energy consumption by
Traditional electric filament lamp and daylight lamp is gradually instead of, the aspects such as illumination and display are mainly used in.In recent years, using rare earth coordination
Macroscopic single crystal goes out the white light emitting material of high energy efficiency and gradually attract attention.Rare earth coordination polymer is a class formation
Novel composite, with various structures, controllability is strong, performance is abundant the features such as.Rare earth element is because have uniqueness
4f configurations, and the property different from other metals is shown, for example：High ligancy, strong coordination ability, from visible region
To the good characteristics of luminescence of infrared light district, long luminescent lifetime etc..Using the unique characteristics of luminescence of rare earth element, binding partner with
The energy transfer existed between rare earth element, different rare earth elements, i.e., so-called " antenna effect ", being expected to synthesize can launch white
The rare earth coordination polymer luminescent material of light.
Because most of rare earth ions have similar chemical property, particularly its ionic radius is close, therefore can be
In same rare earth coordination polymer, by being doped into different types of rare earth ion the knot of coordination polymer is not changed
Structure, by the ratio of different metal ions in regulation product, it is possible to achieve the regulation and control of color, synthesizes ideal white light；
Further, since rare earth coordination polymer luminescent properties additionally depend on organic ligand to ultraviolet or visible ray absorbability, part
Level-density parameter between the effective energy transmission between rare earth ion and rare earth ion, thus want to synthesize high luminance purity,
The rare earth coordination polymer white light emitting material of long life yet suffers from many difficulties, needs to select suitable rare earth metal
Ion and organic ligand, exploration generates the reaction conditions such as suitable temperature, the pH required for title complex.It is of the invention prepared
Compound can be by simply changing Eu3+The ratio of ion, adjusts the luminescent properties of material, obtains white light emitting material, the party
Method is simple, and raw material is easy to get, and possesses certain economic and social benefit.
The content of the invention
It is an object of the invention to provide a kind of rare earth doped coordination polymer as white light emitting material and its preparation
Method, its molecular formula is { [Tb0.695Eu0.305(DHBDC)3(DMF)4](DMF)2}n.The present invention is from containing functionalization hydroxyl base
The organic carboxyl acid part 2,5-Dihydroxyterephthalic acid and rare-earth metal Tb of group3+、Eu3+Ion carries out reaction and prepares rare earth matching somebody with somebody
Compound, by Eu in regulation coordination compound3+Ratio, finally obtain white light emitting material.
For achieving the above object, the present invention is adopted the following technical scheme that：
Described white light emitting material { [Tb0.695Eu0.305(DHBDC)3(DMF)4](DMF)2}nThe preparation method of compound is molten
Agent thermal synthesis method.Weigh the 2,5-Dihydroxyterephthalic acid and the water of 0.0302mmol europium nitrates six, 0.0698mmol of 0.3mmol
The water of Terbium nitrate (Tb(NO3)3) six is added in 23mL politef autoclaves, adds 6mLDMF, is added containing 36wt%-38wt%HCl
Concentrated hydrochloric acid solution, adjusts pH=3.5, and under room temperature 10min is stirred, and the reactor of good seal is put into 120 DEG C of constant temperature two in an oven
My god, then uniform decrease in temperature obtains yellowish-brown bulk crystals in one day to room temperature, and as described coordination polymer, calculation of yield is about
35%（With Eu calculating）.
The white light emitting material is by { [Eu2(DHBDC)3(DMF)4](DMF)2}nIt is rare-earth metal doped in coordination compound
Tb3+Ion, adjusts Eu3+The content of ion, causes organic ligand and Eu3+The change of ionoluminescence intensity, works as Eu3+Ion concentration
For 30.5% when, product can send ideal white light under ultraviolet excitation, and its cie color coordinate is（0.34,0.31).
The present invention remarkable advantage be：
（1）The present invention generates mixing for Tb, Eu mixing with 2,5-Dihydroxyterephthalic acid part and Eu, Tb reacting metal salt
Miscellaneous rare earth coordination polymer, in products therefrom the composition of each rare earth metal close to added raw material ratio, so as to be easy to logical
Cross the ratio of the control each rare earth metal of raw material to adjust the luminescent properties of product；
（2）The present invention adopts solvent-thermal process method, and synthetic method is simple, and product purity is high, and crystalline phase is good；
（3）{[Tb0.695Eu0.305(DHBDC)3(DMF)4](DMF)2}nCompound at room temperature, under the ultraviolet excitation of 370nm
Ideal white light emission can be produced, its cie color coordinate is（0.34,0.31), can be used to prepare new white light
Luminescent material, with good practical value and application prospect.
Description of the drawings
Fig. 1 is gained { [Tb2(DHBDC)3(DMF)4](DMF)2}nLocal structural graph.
Fig. 2 is gained { [Tb2(DHBDC)3(DMF)4](DMF)2}nTomograph.
Fig. 3 is gained { [Tb0.695Eu0.305(DHBDC)3(DMF)4](DMF)2}nEnergy spectrum diagram.
Fig. 4 is gained difference Tb3+/Eu3+{ [the Tb of ratioxEu1-x(DHBDC)3(DMF)4](DMF)2}nPowder diffraction
Figure.
Fig. 5 is different Tb3+/Eu3+{ [the Tb of ratioxEu1-x(DHBDC)3(DMF)4](DMF)2}nInfrared spectrogram.System
Sample loading mode adopts KBr tablettings.
Fig. 6-7 is respectively { [Tb2(DHBDC)3(DMF)4](DMF)2}n{ [Eu2(DHBDC)3(DMF)4](DMF)2}n
Fluorescence spectra under ultraviolet light 370nm is excited in room temperature.
Fig. 8 is different Tb3+/Eu3+{ [the Tb of ratioxEu1-x(DHBDC)3(DMF)4](DMF)2}nUltraviolet light at room temperature
370nm excite under fluorescence spectra.
Fig. 9 difference Tb3+/Eu3+{ [the Tb of ratioxEu1-x(DHBDC)3(DMF)4](DMF)2}n（x=0.5-0.9）And Figure 10
{[Tb0.695Eu0.305 (DHBDC)3(DMF)4](DMF)2}nCie color coordinate diagram under at room temperature ultraviolet light 370nm is excited.
Figure 11 { [Eu2(DHBDC)3(DMF)4](DMF)2}nWith Figure 12 { [Tb0.695Eu0.305(DHBDC)3(DMF)4]
(DMF)2}nFluorescence lifetime figure under at room temperature ultraviolet light 370nm is excited.
Specific embodiment
Embodiment 1
White light emitting material { [Tb0.695Eu0.305(DHBDC)3(DMF)4](DMF)2}nThe preparation of coordination compound.
Weigh the 2,5-Dihydroxyterephthalic acid and the water of 0.0302mmol europium nitrates six, 0.0698mmol nitre of 0.3mmol
The water of sour terbium six, in being added to 23mL politef autoclaves, adds 6mL DMF, adds containing 36wt%-38wt%HCl
Concentrated hydrochloric acid solution, adjusts pH=3.5, and under room temperature 10min is stirred, and the reactor of good seal is put into 120 DEG C of constant temperature two in an oven
My god, then uniform decrease in temperature obtains yellowish-brown bulk crystals in one day to room temperature, and as described coordination polymer, calculation of yield is about
35%（With Eu calculating）.The polymer at room temperature, under the ultraviolet excitation of 370nm, can send white light, and its cie color coordinate is
（0.34,0.31).
Fig. 1 illustrates synthesized { [Tb2(DHBDC)3(DMF)4](DMF)2}nThe partial structurtes of crystal.Wherein, each
Tb3+The oxygen of six carboxyl oxygen atoms and two DMF solvent molecules in ion and five 2,5-Dihydroxyterephthalic acid molecules
Atom forms the polyhedral structure of eight-coordinate.
Fig. 2 is { [Tb2(DHBDC)3(DMF)4](DMF)2}nTomograph, as can be seen from the figure compound tool
There is one-dimensional tunnel structure, duct volume accounts for the 42.8% of total unit cell volume.
Fig. 3 illustrates { [Tb0.695Eu0.305 (DHBDC)3(DMF)4](DMF)2}nMiddle Tb3+And Eu3+Content, both compare
Example is about Tb:Eu= 0.695:0.305, with rate of charge Tb:Eu= 0.698:0.302 coincide substantially.
Fig. 4 is difference Tb3+/Eu3+{ [the Tb of ratioxEu1-x(DHBDC)3(DMF)4](DMF)2}nPowder diagram, from
It can be seen that before and after doping, crystal structure does not occur substantially to change, and remains as pure phase in figure.
Fig. 5 is difference Tb3+/Eu3+{ [the Tb of ratioxEu1-x(DHBDC)3(DMF)4](DMF)2}nInfrared spectrogram, from
Can also prove that the product infrared spectrum before and after adulterating is held essentially constant in figure, the infrared spectrogram of coordination polymer exists
3200cm-1Nearby occur in that the ν of partO-HStretching vibration peak, in 1700 cm-1Nearby there is not characteristic absorption peak, explanation is matched somebody with somebody
Carboxyl oxygen in compound in 2,5-Dihydroxyterephthalic acid sloughs proton and participates in coordination, and hydroxyl oxygen then has neither part nor lot in coordination.
Embodiment 2
Eu in by changing coordination compound3+Content, obtain ideal white light emitting material.
With { [Eu2(DHBDC)3(DMF)4](DMF)2}nFor host material, the Tb of the different proportion that adulterates3+Ion, obtains one
{ [the Tb of seriesxEu1-x(DHBDC)3(DMF)4](DMF)2}nCoordination compound.At room temperature, under the excitation wavelength of ultraviolet light 370nm,
Test fluorescence spectrum, obtains corresponding cie color coordinate.
It is only single metal ion shown in Fig. 6-7（Only contain Eu3+Or Tb3+）Title complex fluorescence spectrum, wherein
Tb- coordination compounds do not show Tb3+The characteristic peak of ion, only part peak it is luminous, after illustrating that part is stimulated, energy is not
Tb can be effectively transferred to3+Ion, i.e., can not be sensitized Tb3+Ionoluminescence.And in the fluorogram of Eu- coordination compounds, both there is Eu3+
The characteristic peak of ion, also show the emission peak of part, and simply part emission peak is weaker, illustrate part to Eu3+Ion is present
Significantly sensibilization.Therefore can be by Eu in regulation coordination compound3+The ratio of ion, changes the relatively strong of two kinds of emission peaks
Degree, and then obtain more satisfactory white light emitting material.
Fig. 8 is Tb in coordination compound3+And Eu3+The molar ratio of ion is respectively from 0.9：0.1 changes to 0.5：0.5 fluorescence
Figure.
Fig. 9-10 can be seen that and carry out obvious color change, with Eu3+Content increase, color is gradually from blueness to white
Color change, Eu3+Molar ratio at 0.5 a little start be partial to yellow, therefore select in Eu3+Molar ratio be 0.5 near
It is adjusted, finds through many experiments, in Tb3+/Eu3+When the molar ratio of ion is 0.695/0.305, generates and compare
Preferable white light emission, its CIE chromaticity coordinates for (0.34,0.31).
Figure 11-12 is respectively { [Eu2(DHBDC)3(DMF)4](DMF)2}n{ [Tb0.695Eu0.305(DHBDC)3(DMF)4]
(DMF)2}nFluorescence lifetime figure.Through calculating, adulterate Tb3+Coordination compound（τ=220ns）Contain Eu more merely3+Coordination compound (τ=
130ns) there is longer fluorescence lifetime.
Form one is { [Tb2(DHBDC)3(DMF)4](DMF)2}nX-ray single crystal diffraction data profile.
Form two is { [Tb2(DHBDC)3(DMF)4](DMF)2}nCrystal structural data in atomic coordinates and equivalent each
To same sex displacement parameter.
Form three is { [Tb2(DHBDC)3(DMF)4](DMF)2}nPart bond distance's bond angle form.
The crystallographic data of the sample crystal structure of form one
The atomic coordinates of the Sample crystals structure of form two（×104）With effective homogeneity displacement parameter（）
Form three is { [Tb2(DHBDC)3(DMF)4](DMF)2}nPart bond distance's bond angle form.
Symmetry operation code in table is as follows：#1 -x,-y,-z; #2 -x,-y-1,-z; #3 -x-1,-y,-z; #4
-x+1,-y+1,-z+1。
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (3)
1. a kind of rare earth doped coordination polymer white light emitting material, it is characterised in that：Its molecular formula is { [Tb0.695Eu0.305
(DHBDC)3(DMF)4](DMF)2}n；Described DHBDC is 2,5-Dihydroxyterephthalic acid；Described DMF be N, N- diformazans
Base Methanamide.
2. a kind of method for preparing rare earth doped coordination polymer white light emitting material as claimed in claim 1, its feature exists
In：Prepared using solvent-thermal process method.
3. method according to claim 2, it is characterised in that：Weigh 0.3mmol2,5- dihydric para-phthalic acids and
The water of 0.0302mmol europium nitrates six, the water of 0.0698mmol Terbium nitrate (Tb(NO3)3)s six are added in the politef autoclave of 23mL,
6mLN, dinethylformamide is added to add the concentrated hydrochloric acid solution containing 36wt%-38wt%HCl, adjust pH=3.5, stir under room temperature
10min is mixed, the reactor of good seal is put into 120 DEG C of constant temperature two days, programmed cooling one day in an oven, obtain yellowish-brown block brilliant
Body, as described coordination polymer.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107556486A (en) * | 2017-08-24 | 2018-01-09 | 中国计量大学 | A kind of rare earth organic framework materials for iron ion fluoroscopic examination and preparation method thereof |
| CN108164716A (en) * | 2018-02-13 | 2018-06-15 | 成都理工大学 | The method for preparing the organic MOFs materials of gadolinium matrix rare earth for white light emission |
| CN110240707A (en) * | 2019-06-10 | 2019-09-17 | 江苏师范大学 | Rear modified metal-organic framework material and the preparation method and application thereof of one kind detection iron ion |
| CN110256687A (en) * | 2019-06-12 | 2019-09-20 | 中国计量大学 | Fluorescent material and the preparation method and application thereof based on rare earth organic framework |
| CN110951084A (en) * | 2018-09-27 | 2020-04-03 | 天津工业大学 | Application of white-light-emitting double-rare-earth metal organic framework material in detection of phenol pollutants |
| CN110951083A (en) * | 2018-09-26 | 2020-04-03 | 天津工业大学 | Double-rare-earth metal organic framework material based on white light emission and preparation method thereof |
| CN113563600A (en) * | 2021-08-15 | 2021-10-29 | 福州大学 | Metal organic framework material with single-component white light characteristic |
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| US11581489B2 (en) | 2019-07-31 | 2023-02-14 | South University Of Science And Technology Of China | White light emitting material, preparation method thereof, and application thereof |
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| CN110256687A (en) * | 2019-06-12 | 2019-09-20 | 中国计量大学 | Fluorescent material and the preparation method and application thereof based on rare earth organic framework |
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| CN113563600A (en) * | 2021-08-15 | 2021-10-29 | 福州大学 | Metal organic framework material with single-component white light characteristic |
| CN115181285A (en) * | 2022-07-12 | 2022-10-14 | 延安大学 | Terbium coordination polymer crystal and preparation method and application thereof |
| CN115404072A (en) * | 2022-08-17 | 2022-11-29 | 浙江理工大学 | Single-phase white light emitting material based on lanthanide metal-organic framework and preparation method thereof |
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