CN102174322A - Novel rare-earth/L type zeolite luminescent material and preparation method thereof - Google Patents
Novel rare-earth/L type zeolite luminescent material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of rare-earth functional materials, and particularly relates to a rare-earth/L type zeolite luminescent material and a preparation method thereof. The material consists of L type zeolite, rare-earth ion (Ln) and bismuth ion, wherein 0.0025 to 0.25mmol of the rare-earth ion and 100mg of zeolite are added, and the mole ratio of the rare-earth ion to the bismuth ion is (1 to 250):(40 to 1). The rare-earth ion (Ln) is Nd3<+>, Sm3<+>, Eu3<+>, Tb3<+>, Ho3<+>, Er3<+>, Yb3<+>, Tm3<+> or Dy3<+>. According to the preparation method, the luminous intensity and the stability of the rare-earth/L type zeolite are enhanced through simple ion exchange and baking processes, and the fluorescence lifetime is greatly improved compared with that of other rare-earth doped zeolite. For example, the excited state lifetime of the L type zeolite luminescent material doped with Eu3<+> is above 1.60ms, the stability is very strong at a high temperature, and remarkably dazzling characteristic glow can be emitted under the ultraviolet irradiation. Based on the characteristics, the rare-earth/L type zeolite luminescent material has strong application values in the aspects of plasma display, illumination, falsification prevention and the like.
Description
Technical field
The invention belongs to the rare earth field of functional materials, be specially a kind of rare earth/zeolite L luminescent material and preparation method thereof.
Background technology
Rare earth element is because unique 4f layer electronic configuration has the potential using value in fields such as metallurgical industry, petrochemical complex, storage hydrogen, glass-ceramic, permanent magnet material, luminescent materials.Eu
3+As the luminescence center of red fluorescence powder, show good luminescent properties, often with
5D
0→
7F
1,2Become main transition.The fluorescent material that contains Eu is at commercial mass production, but shortcoming is the cost costliness, and it is imperative therefore to seek cheap substitute.Yet this substitute must have good optical property, such as can the efficient absorption UV-light at 254nm, and quantum yield higher (＞85%) etc.
In recent years, aluminosilicate zeolite is because of its cheap price, the high thermostability and the good optical transparency and cause people's extensive interest in field of light emitting materials.As, with Eu
3+Be loaded in the y-type zeolite duct by ion exchange method, add organic ligand again: thiophene or 1,10-phenanthroline etc. carries out sensitization to rare earth ion, just can make the luminescent material of excellent performance.
Zeolite L is the aluminosilicate that contains potassium ion, is piled up on the c-direction of principal axis by alternative hexagonal prism cage and cancrinite cage to form, and presses the hexagonal axis rotation again and produces 12 annular distance roads, has one-dimensional tunnel structure, and the aperture is the large micropore molecular sieve of 0.71nm.Not only raw material is cheap for it, is easy to preparation, also has good thermostability, after 800 ℃ of roastings, still keeps original crystalline structure.In addition, zeolite L is the unique up to now aluminosilicate zeolite crystalline microporous material that can realize pattern and granular size finely regulating in the laboratory.Therefore, their the good main body that can be used as light emitting molecule is used for developing multi-functional optical material.For example, professor Calzaferri of Switzerland Bern university develops the supramolecule optical function material of series based on such zeolite, and they are at solar cell, and there is the potential using value in fields such as biological medicine; Obtain the high fluorescent material of thermostability in the zeolite L nano pore of professor Li Huanrong of Hebei University of Technology with the rare earth organic complex loading, they also utilize self-assembling technique that it is assembled into the orderly light-emitting film of structure height.Yet the fluorescence lifetime of such material middle-weight rare earths ion excited state is shorter, and this is attributable in the duct, and the c h bond vibrations dissipate in the hydroxyl and organic ligand.
At present, many both at home and abroad employing high temperature solid-state methods prepare rare earth luminescent material, and this method is the energy consumption height not only, and prepared luminescent material pattern is wayward, occurs sintering phenomenon easily, and above-mentioned shortcoming directly affects the use and the performance of material.The present invention intends developing a kind of have regular pattern, monochromaticity rare earth luminescent material and the preparation method easy, that energy consumption is low thereof preferably.
Summary of the invention
Technical problem to be solved by this invention is: at the complex process that current luminescent material exists, and the preparation temperature height, the big shortcoming that consumes energy provides a kind of novel rare-earth/zeolite L luminescent material and preparation method thereof.This material has advantages such as regular pattern, luminous monochromaticity be good, and it is low that the preparation method has temperature, and energy consumption is low, the manageable advantage of pattern.
The present invention solves this technical problem the technical scheme that is adopted:
A kind of novel rare-earth/zeolite L luminescent material, this material are by zeolite L, and rare earth ion (Ln) and bismuth ion are formed; Its proportioning is: 0.0025-0.25mmol rare earth ion/100mg zeolite, mol ratio rare earth ion: bismuth ion=1～250: 40～1.
Described rare earth ion is (Ln): Nd
3+, Sm
3+, Eu
3+, Tb
3+, Ho
3+, Er
3+, Yb
3+, Tm
3+Or Dy
3+
The preparation method of above-mentioned a kind of rare earth/zeolite L luminescent material, its step is as follows:
(1) with dilute nitric acid dissolution five water Bismuth trinitrate crystal, being mixed with concentration is the 0.01-0.20mol/L bismuth nitrate solution;
(2) be the LnCl of 0.1mol/L with rare earth oxide and concentrated hydrochloric acid compound concentration
3.6H
2O solution;
(3) according to mol ratio Ln: Bi
3+Bismuth nitrate solution and LnCl that=1～250: 40～1 ratio obtains the first step
3.6H
2O solution mixes;
(4) amount according to 0.0025-0.25mmol rare earth ion/100mg zeolite takes by weighing zeolite L, after mixed solution mixes, carries out ion-exchange under 60-100 ℃.
(5) stop ion-exchange behind the 4-48h,, be placed in the baking oven product after the washing dry with deionized water wash step (4) products therefrom.
(6) drying is good product obtains rare earth/zeolite L advanced luminescent material at last at the tubular type kiln roasting.
The invention has the beneficial effects as follows:
1. make the luminous intensity of rare earth/zeolite L and stability strengthen by simple ion exchange process and roasting process.
2. the fluorescence lifetime of rare earth/zeolite L has had greatly raising than other rear-earth-doped zeolites, and for example the product life among the embodiment 5 has reached more than the 1.69ms.
3. there is more intense using value aspects such as at high temperature stability is very strong owing to this kind material, under uviolizing, can send the dazzling characteristic fluorescence of demonstration, and these characteristics make it show at plasma, and are false proof.
Description of drawings
The present invention will be further described below in conjunction with drawings and Examples
Fig. 1 is the excitation-emission spectrum of the embodiment of the invention 1 product rare earth/zeolite L advanced luminescent material.
Fig. 2 is the excitation-emission spectrum of the embodiment of the invention 2 products rare earth/zeolite L advanced luminescent material.
Fig. 3 is the excitation-emission spectrum of the embodiment of the invention 3 products rare earth/zeolite L advanced luminescent material.
Fig. 4 is the stereoscan photograph of the embodiment of the invention 3 products rare earth/zeolite L advanced luminescent material, wherein a is 20000 times of stereoscan photographs of amplification of embodiment 3 products rare earth/zeolite L advanced luminescent material, and b is 50000 times of stereoscan photographs of amplification of embodiment 3 products rare earth/zeolite L advanced luminescent material.
Fig. 5 is the excitation-emission spectrum of the embodiment of the invention 4 products rare earth/zeolite L advanced luminescent material.
Fig. 6 is the excitation-emission spectrum of the embodiment of the invention 5 products rare earth/zeolite L advanced luminescent material.
Fig. 7 is the digital photograph of the embodiment of the invention 5 products rare earth/zeolite L advanced luminescent material under ultraviolet lamp 254nm irradiation.
Embodiment
For clearer explanation the present invention, enumerate following examples, but it there is not any restriction to scope of invention.
According to the document composition length is that (Silke Megelski, Gion Calzaferri (2001) Adv.Funct.Mater11 277-286) as the following zeolite raw material of each embodiment of example, are limited to this but zeolite L required for the present invention is non-for the 64T cylinder zeolite of 1 μ.
Embodiment 1
1. be rare nitric acid that the concentrated nitric acid of 65%-68% is diluted to 2mol/L with concentration, dissolve five water Bismuth trinitrate crystal, be mixed with the Bi (NO of 0.04mol/L with it
3)
3.5H
2O solution.
2. according to 9: 1 volume ratio, with the EuCl of 0.1mol/L
3.6H
2O solution 2.25mL and 0.04mol/LBi (NO
3)
3.5H
2O solution 0.25mL mixes.
3. take by weighing 100mg 64T (being 0.225mmol rare earth ion/100mg zeolite), be placed in the mixed solution, under 80 ℃ temperature, carry out ion-exchange.Refluxed 24 hours.
4. after reaction finishes, the product of usefulness deionized water wash step 3 three times.After centrifugal, put into 80 ℃ of oven dryings, stand-by.
5. dried step 4 product is taken out, after the grinding, place the tubular electric resistance kiln roasting.Temperature rise rate is 2 ℃/min, rises to 700 ℃, is incubated 1.5h again.Promptly make rare earth/zeolite L luminescent material (99mg).
Utilize fluorescence spectrum that embodiment 1 is carried out fluorescence monitoring, monitor collection of illustrative plates as shown in Figure 1:
Excitation spectrum (detection wavelength: 612nm): 200-480nm
Emmission spectrum (excitation spectrum: 395nm): 614nm, 578nm, 592nm, 652nm, 702nm
Life-span: 1.29ms
Embodiment 2
Change the step volume ratio of second among the embodiment 1 into 8: 2, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 2mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.5mL (being 0.2mmol rare earth ion/100mg zeolite).All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.1mg).
Utilize fluorescence spectrum that embodiment 2 is carried out fluorescence monitoring, monitor collection of illustrative plates as shown in Figure 2:
Excitation spectrum (detection wavelength: 612nm): 200-480nm
Emmission spectrum (excitation spectrum: 395nm): 611nm, 576nm, 591nm, 653nm, 703nm
Life-span: 1.29ms
Embodiment 3
Change the step volume ratio of second among the embodiment 1 into 7: 3, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 1.75mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.75mL (being 0.175mmol rare earth ion/100mg zeolite).All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.3mg).
Utilize fluorescence spectrum that embodiment 3 is carried out fluorescence monitoring, monitor collection of illustrative plates as shown in Figure 3:
Excitation spectrum (detection wavelength: 612nm): 200-480nm
Emmission spectrum (excitation spectrum: 395nm): 612nm, 578nm, 593nm, 653nm, 702nm
Life-span: 1.72ms
And embodiment 3 carried out the detection of scanning electron microscope, wherein Fig. 4 a is that enlargement ratio is the stereoscan photograph of rare earth/zeolite L luminescent material of 20000 times, b is that enlargement ratio is the stereoscan photograph of rare earth/zeolite L luminescent material of 50000 times, it shows that the prepared luminescent material of present embodiment does not destroy the basic pattern of zeolite yet under high-temperature roasting, embodied the high thermal resistance of advanced luminescent material.
Embodiment 4
Change the step volume ratio of second among the embodiment 1 into 6: 4, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 1.5mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 1mL (being 0.15mmol rare earth ion/100mg zeolite).All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material.(98.9mg)
Utilize fluorescence spectrum that embodiment 4 is carried out fluorescence monitoring, monitor collection of illustrative plates as shown in Figure 5:
Excitation spectrum (detection wavelength: 612nm): 200-480nm
Emmission spectrum (excitation spectrum: 395nm): 612nm, 578nm, 592nm, 654nm, 702nm
Life-span: 1.77ms
Embodiment 5
Change the step volume ratio of second among the embodiment 1 into 5: 5, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 1.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 1.25mL (being 0.125mmol rare earth ion/100mg zeolite).All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.1mg).
Utilize fluorescence spectrum that embodiment 5 is carried out fluorescence monitoring, monitor collection of illustrative plates as shown in Figure 6:
Excitation spectrum (detection wavelength: 612nm): 200-480nm
Emmission spectrum (excitation spectrum: 395nm): 613nm, 578nm, 592nm, 654nm, 702nm
Life-span: 1.69ms
And under the 254nm irradiation, taken the digital photograph of embodiment 5, and can find out clearly that from Fig. 7 this sample is more even, red vivid, purity of color is very high.
Embodiment 6
Change the step volume ratio of second among the embodiment 1 into 4: 6, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 1mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 1.5mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.2mg).
Embodiment 7
Change the step volume ratio of second among the embodiment 1 into 3: 7, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 0.75mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 1.75mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (97.9mg).
Embodiment 8
Change the step volume ratio of second among the embodiment 1 into 2: 8, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 0.5mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 2mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (98.7mg).
Embodiment 9
Change the step volume ratio of second among the embodiment 1 into 1: 9, promptly add the EuCl of 0.1mol/L
3.6H
2O solution 0.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 2.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (98.4mg).
Embodiment 10
With the step EuCl of second among the embodiment 1
3.6H
2O changes TbCl into
3.6H
2O promptly adds the TbCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (97.5mg).
Embodiment 11
With the step EuCl of second among the embodiment 1
3.6H
2O changes NdCl into
3.6H
2O promptly adds the NdCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (98.2mg).
Embodiment 12
With the step EuCl of second among the embodiment 1
3.6H
2O changes SmCl into
3.6H
2O promptly adds the SmCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.1mg).
Embodiment 13
With the step EuCl of second among the embodiment 1
3.6H
2O changes HoCl into
3.6H
2O promptly adds the HoCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (98.1mg).
Embodiment 14
With the step EuCl of second among the embodiment 1
3.6H
2O changes ErCl into
3.6H
2O promptly adds the ErCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.3mg).
Embodiment 15
With the step EuCl of second among the embodiment 1
3.6H
2O changes YbCl into
3.6H
2O promptly adds the YbCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.4mg).
Embodiment 16
With the step EuCl of second among the embodiment 1
3.6H
2O changes TmCl into
3.6H
2O promptly adds the TmCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (99.5mg).
Embodiment 17
With the step EuCl of second among the embodiment 1
3.6H
2O changes DyCl into
3.6H
2O promptly adds the DyCl of 0.1mol/L
3.6H
2O solution 2.25mL, 0.04mol/L Bi (NO
3)
3.5H
2O solution 0.25mL.All the other processes are all with embodiment 1.Finally make rare earth/zeolite L luminescent material (98.6mg).
As from the foregoing, rare earth/zeolite L luminescent material is all keeping the zeolite good shapes at 800 ℃, so it can be widely used in the stupalith field.This type material has long characteristics of life-span, can be widely used in fluorescence imaging, bio-sensing, fields such as highly sensitive time resolved fluorescence biochemical analysis.
Claims (3)
1. rare earth/zeolite L luminescent material is characterized by this material by zeolite L, and rare earth ion (Ln) and bismuth ion are formed; Its proportioning is: 0.0025-0.25mmol rare earth ion/100mg zeolite, mol ratio rare earth ion: bismuth ion=1～250: 40～1.
2. rare earth as claimed in claim 1/zeolite L luminescent material, it is characterized by described rare earth ion is (Ln): Nd
3+, Sm
3+, Eu
3+, Tb
3+, Ho
3+, Er
3+, Yb
3+, Tm
3+Or Dy
3+
3. the preparation method of rare earth as claimed in claim 1/zeolite L luminescent material, it is as follows to it is characterized by its step:
(1) with dilute nitric acid dissolution five water Bismuth trinitrate crystal, being mixed with concentration is the 0.01-0.20mol/L bismuth nitrate solution;
(2) be the LnCl of 0.1mol/L with rare earth oxide and concentrated hydrochloric acid compound concentration
3.6H
2O solution;
(3) according to mol ratio Ln: Bi
3+Bismuth nitrate solution and LnCl that=1～250: 40～1 ratio obtains the first step
3.6H
2O solution mixes;
(4) amount according to 0.0025-0.25mmol rare earth ion/100mg zeolite takes by weighing zeolite L, after mixed solution mixes, carries out ion-exchange under 60-100 ℃;
(5) stop ion-exchange behind the 4-48h,, be placed in the baking oven product after the washing dry with deionized water wash step (4) products therefrom;
(6) drying is good product obtains rare earth/zeolite L luminescent material at last at the tubular type kiln roasting.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807861A (en) * | 2012-08-20 | 2012-12-05 | 陕西科技大学 | Preparation method for bismuth/montmorillonite photoluminescence material |
| CN103274597A (en) * | 2013-05-21 | 2013-09-04 | 东华大学 | Method for preparing near-infrared luminescent glass by bismuth ion-doped microporous molecular sieve |
| CN105038780A (en) * | 2015-08-14 | 2015-11-11 | 华南理工大学 | Preparation method of bluish violet light-excited red luminescent material |
| CN108893109A (en) * | 2018-08-31 | 2018-11-27 | 上海理工大学 | A kind of divalent europium activates the preparation method of six side's nepheline phase fluorescent materials |
| CN112456792A (en) * | 2020-11-30 | 2021-03-09 | 上海理工大学 | Filter glass for wide-color-gamut display light source and preparation method thereof |
-
2011
- 2011-03-10 CN CN 201110057148 patent/CN102174322B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
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| 李铭岫, 韩占刚: "《稀土氧化物对钼- 铋催化剂性能的影响》", 《稀土》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807861A (en) * | 2012-08-20 | 2012-12-05 | 陕西科技大学 | Preparation method for bismuth/montmorillonite photoluminescence material |
| CN102807861B (en) * | 2012-08-20 | 2014-08-27 | 陕西科技大学 | Preparation method for bismuth/montmorillonite photoluminescence material |
| CN103274597A (en) * | 2013-05-21 | 2013-09-04 | 东华大学 | Method for preparing near-infrared luminescent glass by bismuth ion-doped microporous molecular sieve |
| CN103274597B (en) * | 2013-05-21 | 2015-08-12 | 东华大学 | The method of the near-infrared luminous glass of a kind of bismuth ion doped micropore molecular sieve |
| CN105038780A (en) * | 2015-08-14 | 2015-11-11 | 华南理工大学 | Preparation method of bluish violet light-excited red luminescent material |
| CN108893109A (en) * | 2018-08-31 | 2018-11-27 | 上海理工大学 | A kind of divalent europium activates the preparation method of six side's nepheline phase fluorescent materials |
| CN108893109B (en) * | 2018-08-31 | 2021-04-30 | 上海理工大学 | Preparation method of divalent europium ion activated cancrinite phase fluorescent material |
| CN112456792A (en) * | 2020-11-30 | 2021-03-09 | 上海理工大学 | Filter glass for wide-color-gamut display light source and preparation method thereof |
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