CN106866983A - The regulation and control synthesis of low temperature white light rare earth organic coordination polymer and fluorescence regulation and control - Google Patents
The regulation and control synthesis of low temperature white light rare earth organic coordination polymer and fluorescence regulation and control Download PDFInfo
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Abstract
The invention discloses the preparation method of low temperature white light rare earth organic coordination polymer, part is weighed respectivelyPThe tetrabasic carboxylic acid of terphenyl 2,2,4,4（H4L）, rare-earth salts Eu2(SO4)3 .8H2O, rare-earth salts Tb2(SO4)3 .8H2O, rare-earth salts Dy2(SO4)3 .8H2In vial, four mass ratio is 8 to O:1:1:7, to adding N, N DEFs and distilled water in this mixture, after ultrasonic mixing is uniform, vial is placed in baking oven into 85 DEG C to react 4 days, nature is taken out and is down to room temperature, obtain yellow rhombus transparent crystal, use distilled water flushing crystal, crystal is collected, room temperature is dried, obtained final product.Meanwhile, the invention also discloses the fluorescence regulation and control of low temperature white light rare earth organic coordination polymer.The above-claimed cpd synthetic method that the present invention is provided is simple, and Stability Analysis of Structures can for a long time be placed and preserved in atmosphere.
Description
Technical field
The invention belongs to high molecular polymer field, and in particular to two kinds of low temperature white light mixing-rare earth coordination polymers
Regulation and control synthesis and its fluorescence regulation and control.
Background technology
Controllable luminescent substance has a wide range of applications in the field such as display device and full-color display device.Wherein white light thing
Matter is traditional lighting source material.Traditional white light emitting material is by luminescent substance not of the same race（Such as feux rouges, green glow, blue light）
The mixture of composition.Compared with traditional white light emitting material, various luminous primitives are embedded into the white light formed in single main body
Material all increases significantly in stability, repeatability and combined coefficient.The luminous of lanthanide series has that emission band is narrow, hair
Light long lifespan, it is subject to the extensive concern of researcher the features such as Stokes shift is big.Additionally, the luminous culvert of lanthanide series
Ultraviolet, visible and near infrared region is covered.Extensively with the abundant luminous optimal selection for making lanthanide series turn into luminous primitive, in purple
Under the exciting of outer light, europium element（Eu3+）It is red emission, terbium element（Tb3+）It is green emission, dysprosium element（Dy3+）For orange light is sent out
Penetrate.Metal-organic framework coordination polymer（MOF）Be by metallic element and organoligand coordination formed with three-dimensional structure
Complex, it is simple with synthesis, the features such as structure can be surveyed.This metal-organic coordination polymer can occupy hybrid metal
Metallic site in structure, forms hybrid metal-organic coordination polymer.Therefore, will there are the different group of the lanthanides units for lighting interval
Various rare earth luminous primitives are just embedded into one kind by element simultaneously with organic ligand synthesis mischmetal-organic coordination polymer simultaneously
In light emitting host.The mixing that can just obtain different light emitting regions by the ratio for adjusting different luminescent metal salt in course of reaction is dilute
Soil-organic coordination polymer.
There is the absorption coefficient of light of very little due to rare earth element, so to select suitable organic ligand to come excitation rare-earth unit
Element is luminous in coordination polymer.Bunzli and Latva report that carboxylic acids part has very strong UV Absorption energy in succession
Power, while the luminous energy level of rare earth ion can be transferred energy to, quick magnificent rare earth ion it is luminous.Additionally, according to hard and soft acid and base
Theory, the oxygen atom on carboxylic acid is easier to be coordinated to form rare earth-organic coordination polymer with rare earth element.Therefore mixing dilute
Soil-organic coordination polymer can select multi-carboxylic acid's organic ligand when constructing.
In order to construct white light emitting material, the Eu with red emission is selected3+, green emission Tb3+With orange photoemissive Dy3+
Rare earth element.Can be obtained by changing the luminous intensity of various luminous primitives in rare earth-organic coordination polymer main body
White light emitting material.But energy transfer is commonly present between rare earth element each energy level, this energy transfer is generally by temperature factor
Influence.So such mischmetal-organic coordination polymer it is luminous be influenced by temperature it is larger.But this energy transfer is difficult to
Control, controllable design and the synthesis adjustable white light single main body material of fluorescence is still a kind of challenge in the synthesis of material.
Accordingly, it would be desirable to explore and study luminous influence of the temperature to mischmetal-organic coordination polymer, design synthesis
The research and development of white light parts etc. are had potential application value by the white light emitting material of single main body.
The content of the invention
Goal of the invention：The purpose of the present invention is to solve the shortcomings of the prior art, there is provided low temperature white light rare earth-organic coordination
The regulation and control synthesis of polymer.
Another object of the present invention is to provide low temperature white light rare earth-organic coordination polymer fluorescence regulation and control.
Technical scheme：In order to reach foregoing invention purpose, what the present invention was specifically performed by：A kind of low temperature white light is dilute
Soil-organic coordination polymer (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) preparation method of (DEF), weighs part respectivelyP-
Terphenyl-2,2,4,4-tetrabasic carboxylic acid（H4L）, rare-earth salts Eu2(SO4)3 .8H2O, rare-earth salts Tb2(SO4)3 .8H2O, rare-earth salts Dy2
(SO4)3 .8H2In vial, four mass ratio is 8 to O:1:1:7, to the N that same volume is added in this mixture, N- diethyls
Base formamide and distilled water, N, N- DEF addition isP- terphenyl-2,2,4,4-tetrabasic carboxylic acid quality 5 ~
15%, after ultrasound 10 ~ 20 minutes is well mixed, vial is placed in baking oven 85 DEG C and is reacted 4 days, take out nature and be down to room temperature, obtain
To yellow rhombus transparent crystal, distilled water flushing crystal is used, collect crystal, room temperature is dried, obtained final product.
Another low temperature white light rare earth-organic coordination polymer (Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) (DEF)
Preparation method, weighs part respectivelyP- terphenyl-2,2,4,4-tetrabasic carboxylic acid（H4L）, rare-earth salts Eu2(SO4)3 .8H2O, rare-earth salts
Tb2(SO4)3 .8H2O, rare-earth salts Dy2(SO4)3 .8H2In vial, four mass ratio is 8 to O:1:7:13, to this mixture
The middle N for adding same volume, N- DEFs and distilled water, N, N- DEF addition isP- terphenyl -2,2
, the 5 ~ 15% of 4,4-tetrabasic carboxylic acid quality, after ultrasound is well mixed for 10 ~ 20 minutes, vial is placed on 85 DEG C of reactions 4 in baking oven
My god, take out nature and be down to room temperature, yellow rhombus transparent crystal is obtained, distilled water flushing crystal is used, crystal is collected, room temperature is dried,
Obtain final product.
Wherein, the N, the purity of N- DEFs is more than 99%, and general Reagent Company is commercially available, such as Nanjing
Chemical reagent limited company etc..
Use the fluorescent emission that solid is determined on the Fluorolog-3 XRFs of Horiba Jobin Yvon companies
Spectrum, specific measuring method is as follows：
(Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O)(DEF)：Excited with the ultraviolet light of 336 nm, when temperature is by 300 K
When being cooled to 50 K, due to temperature reduction Tb3+To Eu3+Energy transfer be suppressed, Eu3+Red emission gradually weaken and
Tb3+Green emission gradually reduce, cause the luminous of mischmetal-organic coordination polymer to be sent out by orange gradually changing to white light
Penetrate（Fig. 4）.When temperature drop is to 100 K and 50 K, there is white light emission.The chromaticity coordinates of white light emission is during 100 K（0.32,
0.25）, the chromaticity coordinates of white light emission is when temperature is down to 50K（0.30,0.32）, this chromaticity coordinates with pure white light（0.33,
0.33）Closely；
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O)(DEF)：Excited with the ultraviolet light of 363 nm, when temperature is by 300 K
It is down to 50 K, Eu3+Red emission gradually weaken and Tb3+Green emission gradually reduce, cause mischmetal-organic coordination
The luminous of polymer is gradually changed to white and yellow green by pink colour.（Fig. 5）When temperature drop is to 200 K and 150 K, there is white light
Transmitting.The chromaticity coordinates of white light emission is during 200 K（0.31,0.25）, the chromaticity coordinates of white light emission is when temperature is down to 150K
（0.30,0.30）, this chromaticity coordinates with pure white light（0.33,0.33）Closely.
The invention provides the preparation method of above-claimed cpd, structural characterization, and temperature fluorescence regulation and control method.Obtain two
Mischmetal-the organic coordination polymer of example low temperature white light emission.In addition, the above-claimed cpd synthetic method letter that the present invention is provided
Single, Stability Analysis of Structures can for a long time be placed and preserved in atmosphere.
Beneficial effect：The present invention has advantages below：
（1）The two kinds of low temperature white light mischmetal-organic coordination polymer (Eu for proposing 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O)
And (Eu (DEF) 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) (DEF), is that a class has the mixed rare-earth of brand new-have
Machine coordination polymer, its synthetic method simple and fast, low cost, yield is high, helps lend some impetus to the synthesis of novel coordination polymer
With the research of white light emitting material；
（2）Hybrid metal-organic coordination polymer can be as the main body of the luminous primitive of different rare earth metals, with traditional white light
Mixing material is compared, with certain stability of photoluminescence, while also having repeatability higher；
（3）The two kinds of low temperature white light mischmetal-organic coordination polymer (Eu for proposing 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O)
And (Eu (DEF) 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) (DEF) have air stability very high, moist stability, and
Heat endurance, has expanded the application field of this kind of luminescent material.
Brief description of the drawings
Fig. 1 is shown (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and (Eu 0.0666 Tb 0.4667 Dy 0.4667 )
(HL)(H2O) the powder diffraction spectrum of (DEF)；
Fig. 2 is shown the tomograph of coordination polymer；
Fig. 3 is shown (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and (Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)
(H2O) the thermogravimetry figure of (DEF)；
Fig. 4 is shown the (Eu in the case where the wavelength of 336nm is excited 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) becomes with temperature
The luminescent spectrum and chromaticity coordinates collection of illustrative plates of change；
Fig. 5 is shown the (Eu in the case where the wavelength of 363nm is excited 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) (DEF) becomes with temperature
The luminescent spectrum and chromaticity coordinates collection of illustrative plates of change.
Specific embodiment
Embodiment 1
Low temperature white light mischmetal-organic coordination polymer (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) the synthesis of (DEF)
Part is weighed respectivelyP- terphenyl-2,2,4,4-tetrabasic carboxylic acid（H4L）40 mg, rare-earth salts Eu2(SO4)3 .8H2O 5 mg、
Tb2(SO4)3 .8H2O 5 mg、Dy2(SO4)3 .8H2The mg of O 65 add in the vial that volume is 15 ml in this mixture
Enter 4 ml N, N- DEFs（DEF）With 4 ml distilled water.After ultrasound is well mixed for 15 minutes, reactive material will be contained
Vial be placed in baking oven 85 degrees Celsius and react 4 days.Nature is taken out after four days and is down to room temperature, obtain the transparent crystalline substance of yellow rhombus
Body.Distilled water flushing crystal is used, crystal is collected, room temperature is dried.
Embodiment 2
Low temperature white light mischmetal-organic coordination polymer (Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) the synthesis of (DEF)
Part is weighed respectivelyP- terphenyl-2,2,4,4-tetrabasic carboxylic acid（H4L）40 mg, rare-earth salts Eu2(SO4)3 .8H2O 5 mg、
Tb2(SO4)3 .8H2O 35 mg、Dy2(SO4)3 .8H2The mg of O 35 add in the vial that volume is 15 ml in this mixture
Enter 4 ml N, N- DEFs（DEF）With 4 ml distilled water.After ultrasound is well mixed for 15 minutes, reactive material will be contained
Vial be placed in baking oven 85 degrees Celsius and react 4 days.Nature is taken out after four days and is down to room temperature, obtain the transparent crystalline substance of yellow rhombus
Body.Distilled water flushing crystal is used, crystal is collected, room temperature is dried.
Embodiment 3
Low temperature white light mischmetal-organic coordination polymer (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) Eu in (DEF)3+, Tb3+, and Dy3+The assay of metal
The content of mischmetal-organic coordination polymer Rare Earth Ion is that the Ultima2 for using Jobin Yvon companies feels
Coupled plasma-atomic emission spectrometer is answered to determine two kinds of contents of mischmetal-organic coordination polymer Rare Earth Ion,
Respectively:
(Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O)(DEF)：Eu3+, 2.04%; Tb3+, 2.64%; and Dy3+,
19.27%。
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O)(DEF)：Eu3+, 2.54%; Tb3+, 10.68%; and Dy3+,
11.19%。
Embodiment 4
Low temperature white light mischmetal-organic coordination polymer (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) the Crystal Structure of (DEF)
Two kinds of low temperature white light mischmetal-organic coordination polymer (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) crystal structure of (DEF) and Eu (HL) (H2O) structure of (DEF) is identical.
(Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and (Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) structure of (DEF) is used
X- ray powder diffractions are characterized（Fig. 1）, Eu (HL) (H2O) structure of (DEF) is characterized by X-ray single crystal diffraction.
Test result shows that such coordination polymer has three-dimensional structure（Fig. 2）, rare earth element Eu3+, Tb3+, and Dy3+Can be uniform
It is dispersed at the metallic site of coordination polymer.Such coordination polymer crystallize inP- 1 space group, anorthic system.In structure
There is an Eu in asymmetric cell3+Ion, six from the oxygen atom on part carboxyl oxygen, a N for coordination, N- diethyl
Oxygen atom on the oxygen atom of formamide and a water of coordination.Two adjacent Eu3+Ion is connected by four carboxyl oxygens of bridging
Connect to form two nuclear structure units.This construction unit connects to form three-dimensional structure by four carboxyls on organic ligand.Specific knot
Structure information refers to Cambridge crystal structure database, and No. CCDC is 1496815.Additionally, two coordination polymers can stable existence
In air, with heat endurance very high（Fig. 3）.
Embodiment 5
Low temperature white light mischmetal-organic coordination polymer (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O) (DEF) and
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O) the fluorescence regulation and control of (DEF)
Using the fluorescence emission spectrum that solid is determined on the Fluorolog-3 XRFs of Horiba Jobin Yvon companies,
Specific measuring method is as follows：
(Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O)(DEF)：Excited with the ultraviolet light of 336 nm, when temperature is by 300
When K is cooled to 50 K, due to temperature reduction Tb3+To Eu3+Energy transfer be suppressed, Eu3+Red emission gradually weaken
And Tb3+Green emission gradually reduce, cause the luminous of mischmetal-organic coordination polymer to be gradually changed to white light by orange
Transmitting（Fig. 4）.When temperature drop is to 100 K and 50 K, there is white light emission.The chromaticity coordinates of white light emission is during 100 K（0.32,
0.25）, the chromaticity coordinates of white light emission is when temperature is down to 50K（0.30,0.32）, this chromaticity coordinates with pure white light（0.33,
0.33）Closely.
(Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O)(DEF)：Excited with the ultraviolet light of 363 nm, when temperature by
300 K are down to 50 K, Eu3+Red emission gradually weaken and Tb3+Green emission gradually reduce, cause mischmetal-organic
The luminous of coordination polymer is gradually changed to white and yellow green by pink colour.（Fig. 5）When temperature drop is to 200 K and 150 K, occur
White light emission.The chromaticity coordinates of white light emission is during 200 K（0.31,0.25）, the chromaticity coordinates of white light emission when temperature is down to 150K
For（0.30,0.30）, this chromaticity coordinates with pure white light（0.33,0.33）Closely.
Claims (4)
1. the preparation method of low temperature white light rare earth-organic coordination polymer, it is characterised in that weigh part respectivelyP- terphenyl-
2,2,4,4-tetrabasic carboxylic acid, Eu2(SO4)3 .8H2O、Tb2(SO4)3 .8H2O、Dy2(SO4)3 .8H2O in vial, four quality
Than being 8:1:1:7, to the N that same volume is added in this mixture, N- DEFs and distilled water, N, N- diethyl formyl
Amine addition isP- terphenyl-2, the 5 ~ 15% of 2,4,4-tetrabasic carboxylic acid quality, after ultrasound is well mixed for 10 ~ 20 minutes, by glass
Bottle is placed in baking oven 85 DEG C and reacts 4 days, takes out nature and is down to room temperature, obtains yellow rhombus transparent crystal, brilliant with distilled water flushing
Body, collects crystal, and room temperature is dried, and obtains final product (Eu 0.0667 Tb 0.0667 Dy 0.8666 )(HL)(H2O)(DEF)。
2. the preparation method of low temperature white light rare earth-organic coordination polymer, it is characterised in that weigh part respectivelyP- terphenyl-
2,2,4,4-tetrabasic carboxylic acid, Eu2(SO4)3 .8H2O、Tb2(SO4)3 .8H2O、Dy2(SO4)3 .8H2O in vial, four quality
Than being 8:1:7:13, to the N that same volume is added in this mixture, N- DEFs and distilled water, N, N- diethyl first
Acid amides addition isP- terphenyl-2, the 5 ~ 15% of 2,4,4-tetrabasic carboxylic acid quality, after ultrasound is well mixed for 10 ~ 20 minutes, by glass
Glass bottle is placed in baking oven 85 DEG C and reacts 4 days, takes out nature and is down to room temperature, obtains yellow rhombus transparent crystal, uses distilled water flushing
Crystal, collects crystal, and room temperature is dried, and obtains final product (Eu 0.0666 Tb 0.4667 Dy 0.4667 )(HL)(H2O)(DEF)。
3. the fluorescence regulation and control of low temperature white light rare earth-organic coordination polymer described in claim 1, it is characterised in that use 336 nm
Ultraviolet light excited, when temperature is cooled to 50 K by 300 K, due to temperature reduction Tb3+To Eu3+Energy transfer receive
To suppression, Eu3+Red emission gradually weaken and Tb3+Green emission gradually reduce, cause mischmetal-organic coordination gather
The luminous of compound is gradually changed to white light emission by orange；When temperature drop is to 100 K and 50 K, there is white light emission.
4. the fluorescence regulation and control of low temperature white light rare earth-organic coordination polymer described in claim 2, it is characterised in that use 363 nm
Ultraviolet light excited, when temperature is down to 50 K, Eu by 300 K3+Red emission gradually weaken and Tb3+Green emission
Gradually reduce, cause the luminous of mischmetal-organic coordination polymer to be gradually changed to white and yellow green by pink colour, work as temperature drop
During to 200 K and 150 K, there is white light emission.
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| 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 |
| CN108192111A (en) * | 2018-03-01 | 2018-06-22 | 成都理工大学 | A kind of pyridine acid metalloid organic frame white light emitting material and preparation method thereof |
| CN108329485A (en) * | 2018-04-16 | 2018-07-27 | 天津师范大学 | Double transmitting group of the lanthanides europium metal-organic framework materials and the preparation method and application thereof |
| CN115505132A (en) * | 2022-09-20 | 2022-12-23 | 浙江师范大学 | Dysprosium rare earth-organic framework material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108192111A (en) * | 2018-03-01 | 2018-06-22 | 成都理工大学 | A kind of pyridine acid metalloid organic frame white light emitting material and preparation method thereof |
| CN108192111B (en) * | 2018-03-01 | 2021-07-20 | 成都理工大学 | Pyridine acid metal organic framework white light material and preparation method thereof |
| CN108329485A (en) * | 2018-04-16 | 2018-07-27 | 天津师范大学 | Double transmitting group of the lanthanides europium metal-organic framework materials and the preparation method and application thereof |
| CN115505132A (en) * | 2022-09-20 | 2022-12-23 | 浙江师范大学 | Dysprosium rare earth-organic framework material and preparation method and application thereof |
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