CN105733585B - DS LEuTbH complexs, its nanometer sheet colloidal suspension liquid prepared and preparation method - Google Patents
DS LEuTbH complexs, its nanometer sheet colloidal suspension liquid prepared and preparation method Download PDFInfo
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- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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Abstract
The embodiment of the invention discloses DS LEuTbH complexs, its nanometer sheet colloidal suspension liquid prepared and preparation method, wherein, the chemical composition of the complex is：EuxTb1‑x(OH)2.5DS0.5·nH2O；Wherein, x=0.7 0.9, n=0.5 2.DS LEuTbH complexs provided by the present invention, after being peeled off into nanometer sheet colloidal suspension liquid, the transmitting of white light is realized under the excitation of 284nm wavelength, has filled up the blank for the stratiform rare-earth hydroxide that the unitary system that can send white fluorescent is not present in the prior art；Potential application will be had in terms of fluorescence and colored display.And the preparation method of DS LEuTbH complexs provided by the present invention, simple to operation, mild condition.
Description
Technical field
The present invention relates to lamellar compound field, more particularly to DS-LEuTbH complexs, its nanometer sheet colloidal state prepared is hanged
Supernatant liquid and preparation method.
Background technology
In recent years, inorganic layered compounds are due to its unique main layer board and the tradable characteristic of interlayer anion,
Especially it shows special physicochemical properties after peeling off into single or multiple lift nanometer sheet, and the research for causing people is emerging
Interest.Such as the metal phosphate reported, transition metal dichalcogenide, metal oxide etc., it can be exchanged into by interlayer ion
Larger ion, expands the distance of interlayer, is successfully peeled off, so as to be more conducive to its application.
Rare earth element makes rare earth compound have excellent optics, electricity, magnetics, chemistry because of its unique 4f layer electronics
Property, so as to be widely used in high-performance luminaire, magnetic material, catalyst and other field of functional materials.Stratiform rare earth
Hydroxide (LRHs), general formula Ln8(OH)20(Am-)4/m·nH2O(Ln:Rare earth ion；A:Intercalating ions), main layer board by
Ln3+Form, it is positively charged；Interlayer is made of the anion that can be exchanged with main layer board charge balance.The crystalline substance of LRHs systems
Fluid-structure analysis shows that its main layer board is by 8 coordination dodecahedron [Ln (OH)7H2O] and the 9 coordination leaf-comb anti-prism [Ln in four directions
(OH)8H2O] it is made up of common side, each LnO8Unit and other 2 LnO8And 4 LnO9It is connected, and 8- coordinations and 9- match somebody with somebody
The Local Symmetric center of position is respectively C1And C4v.In rare earth element, especially Eu3+、Tb3+, due to the transition of its internal layer 4f electronics,
Sharp line spectrum is produced, launches obvious red, green light respectively, so as to be widely studied and apply.
But in the prior art, do not have also and utilize Eu3+、Tb3+To prepare the stratiform rare earth that can send white fluorescent
The report of hydroxide.
The content of the invention
The embodiment of the invention discloses DS-LEuTbH complexs, its prepare nanometer sheet colloidal suspension liquid and preparation method,
For filling up the blank for the stratiform rare-earth hydroxide that the unitary system that can send white fluorescent is not present in the prior art.Technology
Scheme is as follows：
The embodiment of the invention discloses DS-LEuTbH complexs, the chemical composition of the complex is：
EuxTb1-x(OH)2.5DS0.5·nH2O；Wherein, x=0.7-0.9, n=0.5-2.
In the preferred embodiment of the present invention, the complex is：
Eu0.8Tb0.2(OH)2.5DS0.5·nH2O。
The embodiment of the invention also discloses the preparation method of foregoing complex, can include：
By water-soluble europium salt, water-soluble terbium salt, lauryl sulfate and hexa rear progress water soluble in water
Thermal response, after reaction, centrifugation, is washed and dry；Wherein, the terbium ion of the europium ion of water-soluble europium salt and water-soluble terbium salt
Molar ratio be 0.7:0.3-0.9:0.1.
In the preferred embodiment of the present invention, the summation and dodecyl sulphur of water-soluble europium salt and water-soluble terbium salt
Hydrochlorate, the molar ratio of hexa are 1：(2-4)：(0.5-2).
In the preferred embodiment of the present invention, the condition of hydro-thermal reaction is：Hydro-thermal reaction 9-16 at 70-100 DEG C
Hour.
In the preferred embodiment of the present invention, the water-soluble europium salt is selected from：EuCl3·6H2O or Eu
(NO3)3·6H2O；The water solubility terbium salt is selected from：TbCl3·6H2O or Tb (NO3)3·6H2O；The lauryl sulfate
For lauryl sodium sulfate.
The embodiment of the invention also discloses nanometer sheet colloidal suspension liquid prepared by the foregoing complex of application.
The embodiment of the invention also discloses the preparation method of nanometer sheet colloidal suspension liquid, and DS-LEuTbH complexs are added
To peeling off in solvent, after being passed through inert gas 10-20 minutes, 60~84h of sealing thermal insulation at a temperature of 35~45 DEG C, obtains nanometer
Piece colloidal suspension liquid.
In the preferred embodiment of the present invention, the stripping solvent is formamide.
In the preferred embodiment of the present invention, the ratio of formamide and DS-LEuTbH complexs is (300-800)
mL/g。
DS-LEuTbH complexs provided by the present invention, after being peeled off into nanometer sheet colloidal suspension liquid, in 284nm ripples
The transmitting of white light is realized under long excitation, the stratiform filled up in the prior art there is no the unitary system that can send white fluorescent is dilute
The blank of native hydroxide；Potential application will be had in terms of fluorescence and colored display.And DS- provided by the present invention
The preparation method of LEuTbH complexs, simple to operation, mild condition.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the XRD diagram of complex prepared by the embodiment of the present invention 1；
Fig. 2 is the fluorescence spectra of complex nanometer sheet colloidal suspension liquid prepared by the embodiment of the present invention 1；
Fig. 3 is the chromaticity coordinates figure of complex nanometer sheet colloidal suspension liquid prepared by 1-3 of the embodiment of the present invention.
Embodiment
DS-LEuTbH complexs provided by the present invention, its chemical composition are EuxTb1-x(OH)2.5DS0.5·nH2O, its
In, DS represents dodecyl sulphate radical ion, and generally between 0.7-0.9, the value range of n is generally the value range of x
0.5-2, is preferably 1-2.
The preparation method of above-mentioned complex can include：
By water-soluble europium salt, water-soluble terbium salt, lauryl sulfate and hexa rear progress water soluble in water
Thermal response, after reaction, centrifuges, washs, dry；Wherein, the terbium ion of the europium ion of water-soluble europium salt and water-soluble terbium salt
Molar ratio be 0.7:0.3-0.9:0.1.Water-soluble europium salt used in the present invention is preferably EuCl3·6H2O or Eu (NO3)3·
6H2O, more preferably EuCl3·6H2O.Water-soluble terbium salt used in the present invention is preferably TbCl3·6H2O or Tb (NO3)3·
6H2O, more preferably TbCl3·6H2O；The lauryl sulfate is preferably lauryl sodium sulfate.It should be noted that
In order to realize the value range of x in prepared complex generally between 0.7-0.9, then need to control europium ion and terbium from
The additional proportion of son, that is, the molar ratio of the europium ion of water-soluble europium salt and the terbium ion of water-soluble terbium salt is 0.7:0.3-
0.9:0.1.Need further exist for illustrating, the centrifugation employed in preparation process, washing and drying process, are that this area is normal
Operation, the present invention is herein without specifically describing.
During actual experiment, the summation and lauryl sulfate, six methylenes of water-soluble europium salt and water-soluble terbium salt
The molar ratio of urotropine is preferably 1：(2-4)：(0.5-2).
The present invention prepares above-mentioned complex by hydro-thermal reaction, and the condition of hydro-thermal reaction can be to add at 70-100 DEG C
When thermal response 9-16 is small.
Nanometer sheet colloidal suspension liquid is prepared using above-mentioned complex, you can realizes white light under the excitation of 284nm wavelength
Transmitting.
Wherein, the chemical composition of the preferable DS-LEuTbH complexs of white light emission effect is：
Eu0.8Tb0.2(OH)2.5DS0.5·nH2O, n=0.5-2.Its preparation method can include：
By water-soluble europium salt, water-soluble terbium salt, lauryl sulfate and hexa rear progress water soluble in water
Thermal response, after reaction, centrifuges, washs, dry；Wherein, the terbium ion of the europium ion of water-soluble europium salt and water-soluble terbium salt
Molar ratio be 0.8：0.2.Water-soluble europium salt used is preferably EuCl3·6H2O or Eu (NO3)3·6H2O, more preferably
EuCl3·6H2O.Water-soluble terbium salt used is preferably TbCl3·6H2O or Tb (NO3)3·6H2O, more preferably TbCl3·
6H2O；The lauryl sulfate is preferably lauryl sodium sulfate.The summation and ten of water-soluble europium salt and water-soluble terbium salt
Dialkyl sulfate, the molar ratio of hexa are preferably 1：(2-4)：(0.5-2).
The method of nanometer sheet colloidal suspension liquid is prepared using above-mentioned complex to be included：The DS- that will be prepared
LEuTbH complexs, which are added to, to be peeled off in solvent, and it is preferably nitrogen after 10-20 minutes to be passed through inert gas, in 35-45 DEG C of temperature
Lower sealing thermal insulation 60-84h (hour), obtains nanometer sheet colloidal suspension liquid.It should be noted that described stripping solvent can be managed
Solve the solvent to enable to above-mentioned complex to form nanometer sheet colloidal suspension liquid in the stripping solvent.For example, bag
Include but be not limited to formamide.
Usually in experimentation, solvent is peeled off, such as the ratio of formamide and DS-LEuTbH complexs can be
(300-800) mL/g, is preferably 500mL/g.
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
1st, Eu is prepared0.8Tb0.2(OH)2.5DS0.5·1.65H2O complexs
By 0.8mmol EuCl3·6H2O and 0.2mmol TbCl3·6H2O, 3mmol SDS (lauryl sodium sulfate),
1mmol HMT (hexa) are added in 100mL water heating kettles, are added 80mL exhaust water, are heated after sealing at 90 DEG C
12h is reacted, is cooled to room temperature, centrifugal treating sample, rotating speed is 15000rpm (rpm), and the time is 3 minutes, through being vented water
After alternately being washed 4 times with absolute ethyl alcohol, it is placed in air and spontaneously dries, obtain the solid powdery complex of 1.8g.
Elemental analyser (the model produced using German Elementar companies：Vario EL) measure the embodiment of the present invention 1
The C of the complex of middle preparation, H content；The plasma inductive coupling produced using PerkinElmer Instrument Ltd. of the U.S.
Atomic Emission Spectrometer AES (ICP) (model：NexION 300X) Eu and Tb of the complex that prepare in the measure embodiment of the present invention 1
Content, it is as a result as shown in the table：
The elemental analysis result of embodiment 1
X-ray powder diffraction instrument (the model produced using Dutch PA Nalytical companies：X Pert PRO MPD) it is right
Obtained Eu0.8Tb0.2(OH)2.5DS0.5·1.65H2O complexs carry out XRD characterization, and the results are shown in Figure 1, a series of from figure
The position of set of diffraction maximum can be seen that the main layer board ordered arrangement of sample, and the feature for all showing layer structure is spread out
Penetrate, its interlamellar spacing isIllustrate the structure of the samples met stratiform rare-earth hydroxide of the synthesis.
2nd, nanometer sheet colloidal suspension liquid is prepared
Complex solid powder prepared by 0.1g embodiments 1 is dispersed in the conical flask for filling 50ml formamides, leads to N2
20 minutes.Then conical flask good seal is stood into insulation 2.5 days in 40 DEG C of insulating boxs, it is about receiving for 2.0g/L to obtain concentration
Rice piece colloidal suspension liquid.
Sepectrophotofluorometer (the model produced using Japanese Shimadzu Corporation：RF-5301PC) to the nanometer sheet glue of preparation
State suspension carries out fluorometric investigation, and Fig. 2 is the emission spectrum under 284nm excitations；Wherein, exciting slit is 5.0nm in test, hair
It is 5.0nm to penetrate slit.
From figure 2 it can be seen that there is Eu in nanometer sheet colloidal suspension liquid3+And Tb3+Characteristic emission.Illustrate Eu3+Success
Ground is mixed with LTbH laminates, meanwhile, it may be seen that being respectively belonging to Tb at 489nm and at 545nm3+Blue green light
And green emission；And it can also be observed that at 613nm, Eu3+Red emission.
Embodiment 2
1st, Eu is prepared0.7Tb0.3(OH)2.5DS0.5·1.37H2O complexs
By 0.7mmol EuCl3·6H2O and 0.3mmol TbCl3·6H2O, 3mmol SDS (lauryl sodium sulfate),
1mmol HMT (hexa) are added in 100mL water heating kettles, are added 80mL exhaust water, are heated after sealing at 70 DEG C
16h is reacted, is cooled to room temperature, centrifugal treating sample, rotating speed 15000rpm, the time is 3 minutes, through being vented water and absolute ethyl alcohol
After alternately washing 4 times, it is placed in air and spontaneously dries, obtain the complex of 1.8g.
The elemental analysis result of embodiment 2
2nd, nanometer sheet colloidal suspension liquid is prepared
Complex solid powder prepared by 0.1g embodiments 2 is dispersed in the conical flask for filling 50ml formamides, leads to N2
10min.Then conical flask good seal is stood into insulation 2.5 days in 40 DEG C of insulating boxs, it is about receiving for 2.0g/L to obtain concentration
Rice piece colloidal suspension liquid.
Embodiment 3
1st, Eu is prepared0.9Tb0.1(OH)2.5DS0.5·1.61H2O complexs
By 0.9mmol EuCl3·6H2O and 0.1mmol TbCl3·6H2O, 3mmol SDS (lauryl sodium sulfate),
1mmol HMT (hexa) are added in 100mL water heating kettles, are added 80mL exhaust water, are heated after sealing at 100 DEG C
9h is reacted, is cooled to room temperature, centrifugal treating sample, rotating speed 15000rpm, the time is 3 minutes, through being vented water and absolute ethyl alcohol
After alternately washing 4 times, it is placed in air and spontaneously dries, obtain the complex of 1.8g.
The elemental analysis result of embodiment 3
2nd, nanometer sheet colloidal suspension liquid is prepared
Complex solid powder prepared by 0.1g embodiments 3 is dispersed in the conical flask for filling 50ml formamides, leads to N2
20min.Then conical flask good seal is stood into insulation 2.5 days in 40 DEG C of insulating boxs, it is about receiving for 2.0g/L to obtain concentration
Rice piece colloidal suspension liquid.
Fluorometric investigation
Nanometer sheet colloidal suspension liquid prepared by embodiment 1-3 is subjected to fluorometric investigation respectively, obtains chromaticity coordinates figure, is such as schemed
Shown in 3, from figure 3, it can be seen that the nanometer sheet colloidal suspension liquid prepared by embodiment 1-3, in x=0.7,0.8 and 0.9
Chromaticity coordinates is respectively (0.34,0.38), and (0.36,0.35) and (0.37,0.32), illustrates that the nanometer sheet colloidal state of three kinds of synthesis is hanged
Supernatant liquid is in the range of white light area, it is possible to achieve the transmitting of white light；During wherein x=0.8 with optimal white point (0.33,0.33) most
Close, white light emission effect is more preferable.
Above to DS-LEuTbH complexs provided by the present invention, its nanometer sheet colloidal suspension liquid prepared and preparation side
Method is described in detail.Specific embodiment used herein is set forth the principle of the present invention and embodiment, with
The explanation of upper embodiment is only intended to help the method and its central idea for understanding the present invention.It should be pointed out that for this area
For those of ordinary skill, without departing from the principle of the present invention, some improvement and modification can also be carried out to the present invention,
These are improved and modification is also fallen into the protection domain of the claims in the present invention.
Claims (9)
1.DS-LEuTbH complexs, it is characterised in that the chemical composition of the complex is：
Eu0.8Tb0.2(OH)2.5DS0.5·nH2O；Wherein DS represents dodecyl sulphate radical ion, n=0.5-2.
2. the preparation method of complex described in claim 1, it is characterised in that including：
Water-soluble europium salt, water-soluble terbium salt, lauryl sulfate and hexa rear progress hydro-thermal soluble in water is anti-
Should, after reaction, centrifugation, is washed and dry；Wherein, the europium ion of water-soluble europium salt and the terbium ion of water-soluble terbium salt rub
You are than being 0.7:0.3-0.9:0.1.
3. preparation method as claimed in claim 2, it is characterised in that the summation and 12 of water-soluble europium salt and water-soluble terbium salt
Alkyl sulfate, the molar ratio of hexa are 1：(2-4)：(0.5-2).
4. preparation method as claimed in claim 2, it is characterised in that the condition of hydro-thermal reaction is：Hydro-thermal is anti-at 70-100 DEG C
When answering 9-16 small.
5. such as the preparation method any one of claim 2-4, it is characterised in that the water solubility europium salt is selected from：
EuCl3·6H2O or Eu (NO3)3·6H2O；The water solubility terbium salt is selected from：TbCl3·6H2O or Tb (NO3)3·6H2O；Institute
It is lauryl sodium sulfate to state lauryl sulfate.
A kind of 6. nanometer sheet colloidal suspension liquid prepared by complex using described in claim 1.
7. the preparation method of the nanometer sheet colloidal suspension liquid described in claim 6, it is characterised in that by DS-LEuTbH complexs
It is added to and peels off in solvent, after being passed through inert gas 10-20 minutes, when sealing thermal insulation 60~84 is small at a temperature of 35~45 DEG C,
Obtain nanometer sheet colloidal suspension liquid.
8. preparation method as claimed in claim 7, it is characterised in that the stripping solvent is formamide.
9. preparation method as claimed in claim 8, it is characterised in that the ratio of formamide and DS-LEuTbH complexs is (300-
800)mL/g。
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| CN102050920A (en) * | 2010-10-30 | 2011-05-11 | 太原理工大学 | Synthesis method of macromolecular white light phosphor powder containing europium and terbium |
| CN102268252A (en) * | 2011-06-15 | 2011-12-07 | 北京师范大学 | 4-biphenyl formate/YEu-LRH (layered rare-earth hydroxide) organic compound and synthesis method thereof |
| CN102585813A (en) * | 2011-12-28 | 2012-07-18 | 大连海事大学 | Color-controllable long afterglow material excited by ultraviolet light and preparation method thereof |
| CN105238386A (en) * | 2014-08-18 | 2016-01-13 | 阜阳师范学院 | Method for preparing rare earth complex-doped fluorescent powder |
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Patent Citations (4)
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|---|---|---|---|---|
| CN102050920A (en) * | 2010-10-30 | 2011-05-11 | 太原理工大学 | Synthesis method of macromolecular white light phosphor powder containing europium and terbium |
| CN102268252A (en) * | 2011-06-15 | 2011-12-07 | 北京师范大学 | 4-biphenyl formate/YEu-LRH (layered rare-earth hydroxide) organic compound and synthesis method thereof |
| CN102585813A (en) * | 2011-12-28 | 2012-07-18 | 大连海事大学 | Color-controllable long afterglow material excited by ultraviolet light and preparation method thereof |
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| Structural and photoluminescent investigation of LTbH/LEuH nanosheets and their color-tunable colloidal hybrids;Yushuang Zhao et al.;《Journal of materials chemistry C》;20130411;第1卷;3584-3592 * |
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