CN103694991B - Novel color-adjusted rare earth luminous material and preparation method thereof - Google Patents
Novel color-adjusted rare earth luminous material and preparation method thereof Download PDFInfo
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- CN103694991B CN103694991B CN201310644088.6A CN201310644088A CN103694991B CN 103694991 B CN103694991 B CN 103694991B CN 201310644088 A CN201310644088 A CN 201310644088A CN 103694991 B CN103694991 B CN 103694991B
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Abstract
The invention discloses a novel color-adjusted rare earth luminous material. The rare earth luminous material comprises amino clay, pyromellitic sodium formate and trivalent rare earth element ions, wherein the amount ratio of the amino clay to the pyromellitic sodium formate is 13:7; the amount ratio of the pyromellitic sodium formate (ligand) to the trivalent rare earth element ions (central ions) is 3:4. An organic ligand pyromellitic sodium formate is introduced into the amino clay in a mode of combining the cation and anion, and ligand can be coordinated with the rare earth ions. The obtained rare earth luminous material is cheap and readily available in raw materials, simple in preparation method, environment-friendly and high in plasticity, has high fluorescence intensity, high optical stability and long fluorescent lifetime of 0.37-1.00ms, can emit colorful fluorescence by adjusting the types and content of the rare earth ions and can be used for manufacturing optical devices and luminous films.
Description
Technical field
The present invention is subordinate to rare earth luminescent material field, is specially adjustable novel rare-earth luminescent material of a kind of color and preparation method thereof.
Technical background
Stratiform is similar 2:1 type trioctahedron layered silicate (polynite) in a kind of structure containing magnesium nanoclay, with talcum [Si
8mg
6o
20(OH)
4] be the novel artificial synthesis of clay of parent, molecular formula is R
8si
8mg
6o
16(OH)
4.Amino clay is the most representative a kind of in this class clay, and its R base is-(CH
2)
3nH
2, molecular weight is 1156, between lamella, by Intermolecular Forces, is arranged in parallel, and has formed the laminate structure of spacial ordering, interlamellar spacing (width between centerss of two parallel lamellas) is about 1.7nm.A critical nature of amino clay, is that its amino can make its each lamella all positively charged in conjunction with proton in water, thereby makes between lamella the peeling off phenomenon due to the effect of coulomb repulsion, finally in water, disperses completely, forms colloidal sol; If add carboxylate salt, due to electrical neutralization, clay layer can be recombinated in conjunction with this carboxylate salt, forms gel.Utilize this character of amino clay, can to it, modify by sol-gel method, thereby obtain the gel of desired properties.
Rare earth element luminous is the transition within f-f configuration or between f-d configuration of 4f electronics based on them.Rare earth atom or the ion with the 4f shell of underfilling, nearly more than 20 ten thousand, its energy level transition passage, by the suitable hertzian wave that can launch from ultraviolet to infrared various wavelength that excites, be huge " a luminous treasure-house ", in fields such as information technology, biotechnology, energy technology and science and techniques of defence, having high using value, is a kind of important strategic resource.
Rare earth element and suitable organic ligand, in conjunction with the title complex forming, have extinction ability strong, the abundant and purity of color advantages of higher of fluorescent color, in field of light emitting materials, there is extremely important status, but its shortcoming is unstable to light and heat, easily decompose, cause its application to be subject to certain limitation.Amino clay is as a kind of inorganic matrix, and its light, heat, chemical stability are higher, have good workability, and environmental protection, are the ideal carriers of rare earth organic complex.
In recent years, the research of the properties and applications of relevant amino clay increases gradually, in the achievement in research of field of light emitting materials, be also reported in media, but and the correlative study achievement of rare earth compounding combination also do not appear in one's mind.The present invention is intended to by sol-gel method organic ligand and amino clay in conjunction with forming gel, more further with rare earth ion in conjunction with obtaining rare earth luminescent material, there is raw material and be cheaply easy to get, the advantage such as reaction conditions is gentle, easy and simple to handle, environmentally friendly.
Summary of the invention
The object of the invention is: the preparation method that the adjustable novel rare-earth luminescent material of a kind of color is provided.The method is first by the water-soluble formation colloidal sol of amino clay of preparing in advance, then add wherein the Pyromellitic Acid sodium water solution of finite concentration and volume to make gel, again by gained gel and trivalent rare earth element ionic bond, and by regulating the contamination of trivalent rare earth element ion, obtain the adjustable novel rare-earth luminescent material of color.
Technical scheme of the present invention is:
The novel rare-earth luminescent material that color is adjustable, the composition of this rare earth luminescent material comprises amino clay, Pyromellitic Acid sodium and trivalent rare earth element ion; Wherein, the ratio of the amount of substance of amino clay and Pyromellitic Acid sodium is 13:7; The ratio of the amount of substance of Pyromellitic Acid sodium (part) and trivalent rare earth element ion (central ion) is 3:4.
Described rare earth element is specially: one or more in Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm and Yb.
Wherein, the unit structure type of described amino clay is as follows:
The preparation method of the novel rare-earth luminescent material that described color is adjustable comprises the steps:
(1) by Magnesium dichloride hexahydrate (MgCl
26H
2o) under agitation condition, be dissolved in dehydrated alcohol, again γ-aminopropyl triethoxysilane (APTES) is dropwise joined in reaction system, at room temperature stir 24h, obtain white emulsion, then centrifugal treating abandoning supernatant, obtain white jelly, with this jelly of absolute ethanol washing 2～3 times, in 80 ℃ of air dryings, finally use mortar porphyrize, obtain amino clay; Wherein, material proportion is that quality is than Magnesium dichloride hexahydrate (MgCl
26H
2o): γ-aminopropyl triethoxysilane (APTES)=1.68:2.5, every 50mL dehydrated alcohol adds 1.68g Magnesium dichloride hexahydrate;
(2) get amino clay, adding distilled water dissolves, add again 70mmol/L Pyromellitic Acid sodium water solution, there is white jelly, stir to mix, then add the rare earth chloride ethanolic soln of 93.35mmol/L, stir and supersound process, in 80 ℃ of air dryings, finally use mortar porphyrize, obtain the adjustable novel rare-earth luminescent material of color; Wherein, material proportion is volume ratio distilled water: Pyromellitic Acid sodium water solution: rare earth chloride ethanolic soln=0.34:0.40:0.40, the amino clay of every 0.0601g adds 0.34mL distilled water.
Described rare earth chloride is specially NdCl
3, SmCl
3, EuCl
3, GdCl
3, TbCl
3, D
ycl
3, HoCl
3, ErCl
3, TmCl
3and YbCl
3in one or more.
Beneficial effect of the present invention is:
(1) in amino clay, in the mode of zwitterion combination, introduce organic ligand Pyromellitic Acid sodium, can carry out coordination with rare earth ion.By amino clay gel rare earth compounding fluorescence emission spectrum, can see the characteristic peak of rare earth ion, the ligand structure coordination success in rare earth ion and amino clay gel is described.
(2) the rare earth luminescent material raw material of gained of the present invention is cheaply easy to get, preparation method is simple, environmentally friendly, plasticity-is strong, has higher fluorescence intensity, good light stability, fluorescence lifetime is grown (0.37-1.00ms), and can, by regulating kind and the content of rare earth ion to send colourful fluorescence, be of very high actual application value, can be used for making optics, light-emitting film etc.
Accompanying drawing explanation
Fig. 1 is the fluorescent exciting spectrogram of the amino clay gel europium complex in embodiment 1;
Fig. 2 is the fluorescence emission spectrogram of the amino clay gel europium complex in embodiment 1;
Fig. 3 is the fluorescence lifetime figure of the amino clay gel europium complex in embodiment 1;
Fig. 4 is the fluorescent exciting spectrogram of the amino clay gel terbium coordination compound in embodiment 2;
Fig. 5 is the fluorescence emission spectrogram of the amino clay gel terbium coordination compound in embodiment 2;
Fig. 6 is the fluorescence lifetime figure of the amino clay gel terbium coordination compound in embodiment 2;
Fig. 7 is the amino clay gel europium/terbium coordination compound resulting fluorescence emission spectrogram under 325nm ultraviolet excitation in embodiment 3;
Fig. 8 is the amino clay gel europium/terbium coordination compound resulting fluorescence emission spectrogram under 325nm ultraviolet excitation in embodiment 4;
Embodiment
For clearer explanation the present invention, enumerate following examples, but it is without any restrictions to scope of invention.
The modular construction of the amino clay the present invention relates to is shown below: (amino clay molecules formula [(CH
2)
3nH
2]
8si
8mg
6o
16(OH)
4, molecular weight 1156)
Its preparation method is known technology, its preparation method is shown in document K.K.R.Datta, A.Achari and M.Eswaramoorthy.Aminoclay:A Functional Layered Material With Multifaceted Applications.J.Mater.Chem.A, 2013, the interlamellar spacing of the amino clay of 1,6707 – 6718. gained is about 1.7nm.
Embodiment 1
1. get 1.68g Magnesium dichloride hexahydrate (MgCl
26H
2o, commercially available), under agitation condition, be dissolved in 50mL dehydrated alcohol, get 2.5g γ-aminopropyl triethoxysilane (APTES, commercially available) dropwise join in reaction system, at room temperature (20～25 ℃) stir 24h, and reaction solution is carried out to centrifugal treating abandoning supernatant, obtain white jelly, with this jelly of absolute ethanol washing 2～3 times, in 80 ℃ of air dryings, finally use mortar porphyrize, obtain amino clay.
2. get the amino clay of 0.0601g, add 0.34mL distilled water to dissolve, then add 0.40mL70mmol/L Pyromellitic Acid sodium water solution, occur white jelly, stir to mix, then add the EuCl of 0.40mL93.35mmol/L
3ethanolic soln, stirs and supersound process, in 80 ℃ of air dryings, finally uses mortar porphyrize, obtains amino clay gel europium complex luminescent material.
Utilize fluorescence spectrophotometer to measure the luminescent properties of this amino clay gel europium complex (as excitation spectrum, emmission spectrum and fluorescence lifetime etc.).
Fig. 1-3 are fluorescence excitation spectrum (612nm is for detecting wavelength), fluorescence emission spectrum (300nm is for detecting wavelength) and the fluorescence lifetime figure of amino clay gel europium complex.Title complex has a wide absorption peak within the scope of 230nm-330nm as shown in Figure 1, and maximum excitation wavelength is 300nm; As seen from Figure 2, title complex has 5 emission peaks at 579nm, 592nm, 612nm, 650nm and 700nm place, respectively corresponding Eu
3+?
5d
0→
7f
jthe transition that (J=0,1,2,3,4) locates, wherein with transition
5d
0→
7f
2(612nm) red emission intensity is maximum, the part success coordination in europium ion and gel is described, and has launched its red characteristic fluorescence under certain condition; It is 0.37ms that extinction curve in Fig. 3 carries out the fluorescence lifetime that single index matching can this gel europium complex.
Embodiment 2
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the TbCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel terbium coordination compound luminescent material.
Fig. 4-6 are fluorescence excitation spectrum (544nm is for detecting wavelength), fluorescence emission spectrum (300nm is for detecting wavelength) and the fluorescence lifetime figure of amino clay gel europium complex.Title complex has a wide absorption peak within the scope of 230nm-330nm as shown in Figure 4, and maximum excitation wavelength is 300nm; As seen from Figure 5, title complex has 4 emission peaks at 490nm, 544nm, 584nm and 620nm place, respectively corresponding Tb
3+?
5d
4→
7f
jthe transition that (J=6,5,4,3) locates, wherein with transition
5d
4→
7f
5(544nm) green emission intensity is maximum, the part success coordination in terbium ion and gel is described, and has launched its green characteristic fluorescence under certain condition; It is 1.00ms that extinction curve in Fig. 6 carries out the fluorescence lifetime that single index matching can this gel terbium coordination compound.
Embodiment 3
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the EuCl of 0.05mL93.35mmol/L in step 2
3the TbCl of ethanolic soln and 0.35mL93.35mmol/L
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel europium/terbium coordination compound luminescent material (ratio of the amount of substance of europium and terbium is 1:7).
Fig. 7 is the amino clay gel europium/terbium coordination compound of gained resulting fluorescence emission spectrogram under 325nm ultraviolet excitation.As seen from Figure 7, at 612nm and 544nm place, there are two climaxs, respectively corresponding Eu
3+and Tb
3+characteristic emission peak, the part coordination success in visible rare earth ion and gel.This title complex can send purer white light under 325nm ultraviolet excitation, and it is (0.3421,0.3374) corresponding to the coordinate point on CIE1931 chromaticity diagram, and white light ideal point (0.3333,0.3333) is very approaching.
Embodiment 4
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the EuCl of 0.02mL93.35mmol/L in step 2
3the TbCl of ethanolic soln and 0.38mL93.35mmol/L
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel europium/terbium coordination compound luminescent material (ratio of the amount of substance of europium and terbium is 1:19).
Fig. 8 is the amino clay gel europium/terbium coordination compound of gained resulting fluorescence emission spectrogram under 325nm ultraviolet excitation.As seen from Figure 8, at 612nm and 544nm place, there are two climaxs, respectively corresponding Eu
3+and Tb
3+characteristic emission peak, the part coordination success in visible rare earth ion and gel.This title complex also can send purer white light under 325nm ultraviolet excitation, and it is (0.3362,0.3544) corresponding to the coordinate point on CIE1931 chromaticity diagram, and white light ideal point (0.3333,0.3333) is also more approaching.
Embodiment 5
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the NdCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel neodymium complex luminescent material.
Embodiment 6
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the ErCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel erbium complex luminescent material.
Embodiment 7
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the GdCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel Gd coordination compound luminescent material.
Embodiment 8
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the DyCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel dysprosium complex luminescent material.
Embodiment 9
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the HoCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel holmium complex luminescent material.
Embodiment 10
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the SmCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel samarium complex luminescent material.
Embodiment 11
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the TmCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel thulium complex luminescent material.
Embodiment 12
Step 1, with embodiment 1 step 1, only need change the rare earth compounding solution in embodiment 1 step 2 into the YbCl of 93.35mmol/L in step 2
3ethanolic soln, other conditions are constant.Finally can obtain amino clay gel ytterbium complex luminescent material.
Claims (2)
1. the adjustable novel rare-earth luminescent material of color, the composition that it is characterized by this rare earth luminescent material comprises amino clay, Pyromellitic Acid sodium and trivalent rare earth element ion; Wherein, the ratio of the amount of substance of amino clay and Pyromellitic Acid sodium is 13:7; The ratio of the amount of substance of Pyromellitic Acid sodium (part) and trivalent rare earth element ion (central ion) is 3:4;
Wherein, the modular construction of described amino clay is shown below:
Described rare earth element is specially: one or more in Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm and Yb.
2. the preparation method of the adjustable novel rare-earth luminescent material of color as claimed in claim 1, is characterized by and comprise the steps:
(1) by Magnesium dichloride hexahydrate (MgCl
26H
2o) under agitation condition, be dissolved in dehydrated alcohol, again γ-aminopropyl triethoxysilane (APTES) is dropwise joined in reaction system, at room temperature stir 24h, obtain white emulsion, then centrifugal treating abandoning supernatant, obtain white jelly, with this jelly of absolute ethanol washing 2 ~ 3 times, in 80 ℃ of air dryings, finally use mortar porphyrize, obtain amino clay; Wherein, material proportion is that quality is than Magnesium dichloride hexahydrate (MgCl
26H
2o): γ-aminopropyl triethoxysilane (APTES)=1.68:2.5, every 50mL dehydrated alcohol adds 1.68g Magnesium dichloride hexahydrate;
(2) get amino clay, adding distilled water dissolves, add again 70mmol/L Pyromellitic Acid sodium water solution, there is white jelly, stir to mix, then add the rare earth chloride ethanolic soln of 93.35mmol/L, stir and supersound process, in 80 ℃ of air dryings, finally use mortar porphyrize, obtain the adjustable novel rare-earth luminescent material of color; Wherein, material proportion is volume ratio distilled water: Pyromellitic Acid sodium water solution: rare earth chloride ethanolic soln=0.34:0.40:0.40, and the amino clay of every 0.0601g adds 0.34mL distilled water;
Described rare earth chloride is specially NdCl
3, SmCl
3, EuCl
3, GdCl
3, TbCl
3, DyCl
3, HoCl
3, ErCl
3, TmCl
3and YbCl
3in one or more.
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| CN103937493B (en) * | 2014-05-12 | 2016-01-06 | 福建师范大学 | A kind of preparation method of white light polynite fluorescent material of ultraviolet excitation |
| CN106939163B (en) * | 2017-03-13 | 2019-04-09 | 吉林大学 | A kind of preparation method of the fluorescent functional organic clay of height water dispersible |
| CN113429964A (en) * | 2021-06-25 | 2021-09-24 | 南京信息工程大学 | Preparation method of fluorescent amino clay |
| CN115044363A (en) * | 2022-06-17 | 2022-09-13 | 山东大学 | Preparation method of wormlike micelle-based rare earth element-containing compound luminescent fluid |
| CN117659997B (en) * | 2024-02-02 | 2024-04-02 | 德州学院 | Organic-inorganic hybridization rare earth luminous hydrogel and preparation method and application thereof |
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