CN103923645A - Method for preparing one-dimensional SiO2:Eu<3+>, Gd<3+> nano luminescent material with controllable morphology - Google Patents
Method for preparing one-dimensional SiO2:Eu<3+>, Gd<3+> nano luminescent material with controllable morphology Download PDFInfo
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- CN103923645A CN103923645A CN201410188084.6A CN201410188084A CN103923645A CN 103923645 A CN103923645 A CN 103923645A CN 201410188084 A CN201410188084 A CN 201410188084A CN 103923645 A CN103923645 A CN 103923645A
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Abstract
The invention provides a method for preparing a one-dimensional SiO2:Eu<3+>, Gd<3+> nano luminescent material with controllable morphology, and belongs to the field of preparation technology of inorganic materials. A method combining sol-gel synthesis with calcination process is adopted in the invention to successfully prepare a one-dimensional SiO2 nanomaterial with rod-shaped morphology and co-doped with europium and gadolinium. Red light emitted by the prepared one-dimensional silica nanorod nano luminescent material belongs to 5D0-7D2 transition of a Eu<3+> ion, the Gd<3+> corresponds to sharp line emission of 6P7/2 to 8S7/2 transition at 314 nm, and SiO2:Eu<3+> luminescence has good monochromaticity. The method provided by the invention is strong in operability, mild in reaction conditions and good in reproducibility, and the structure of the obtained product is stable, so that the method is a feasible method used for preparing a red luminescent material with high luminous efficiency and good monochromaticity.
Description
Technical field
The invention belongs to inorganic materials preparing technical field, be specifically related to the controlled one dimension SiO of pattern of a kind of europium, gadolinium codoped
2the preparation method of nano luminescent material.
Background technology
In recent years, there is special appearance, size adjustable micro-nanometer structural material has great importance in basic scientific research and practical application, be subject to people and paid close attention to widely.Monodimension nanometer material, as nanometer rod and nanotube etc., in the widespread use in the fields such as optical material, pharmaceutical carrier and biosensor, has caused and has paid close attention to widely and study.The character of monodimension nanometer material not only depends on its composition, is also subject to the impact of its structure, pattern, size and spatial arrangement etc.Monodimension nanometer material, is used in upper dimension bound transport phenomena processed, has potential application in a lot of fields simultaneously.Rare earth element 4f electron structure is special, and its photoluminescent property has narrowband emission, luminous efficiency and is not subject to the features such as rare earth ion surrounding environment influence and stable in properties.Rare earth mixing with nano material is the high performance luminescent material of a class, has a extensive future in Application Areass such as biosensor, cell imaging and organic electroluminescent LEDs.Along with the development of solid laser material and advanced luminescent material, utilizing sol-gel method to prepare silicon-dioxide luminescent material becomes the focus of research, in silicon-dioxide, will greatly improve luminescent properties by rare earth ion doped.
Transmission ofenergy is the important channel of improving luminous efficiency.Choose Gd
3+for rare-earth ion-doped altogether, as sensitizing agent, Eu
3+as activator ion, because Gd
3+can absorb again or self-energy is effectively passed to luminescence center sensitization Eu by the mode such as resonant energy transfer by photon
3+.Gd
3+be a kind of important rare earth ion, its optical transition occurs in 4f shell, is transmitted in ultraviolet region.Energy difference between its first excited state and ground state level is greater than 3200cm
-1, maximum absorption and transferring energy effectively in trivalent rare earth ions, therefore can be used as good sensitizing agent.
Existing rear-earth-doped one dimension SiO
2the preparation method of nanometer rod is for several below: (1) solvent thermal synthesis method (Ziwei Tang, Liqun Zhou, Lan Yang, Fen Wang, Journal of Luminescence, Volume130, Issue1, Januar
y2010, Pages45 – 51); (2) sol-gel method (Bing Hu and Jianlin Shi (2003) J.Mater.Chem., 2003,13,1250 – 1252); (3) hydrothermal method (Jia G, Liu K, Zheng YH, Song YH, Yang M, You HP, J.Phys.Chem.C, 2009,113 (15), pp6050 – 6055), wherein solvent thermal synthesis method and hydrothermal method generally need the condition of High Temperature High Pressure, harsher, and the reaction conditions of sol-gel method is comparatively gentle.
Summary of the invention
The object of the invention is the method that adopts sol-gel synthesis to combine with calcination process, prepare a kind of one dimension SiO
2: Eu
3+, Gd
3+nano luminescent material, described one-dimentional structure is nanometer rod, its step is as follows:
(1) 0.20～0.35g tensio-active agent cetyl trimethylammonium bromide (CTAB) and 0.03～0.07g dispersion agent polyoxyethylene glycol (PEG-2000) are dissolved in 30～70mL deionized water, and are positioned over and in 30 DEG C～80 DEG C water-baths, are stirred to tensio-active agent and dissolve completely;
(2) by 1～3mL ammoniacal liquor (NH
4oH) be slowly added drop-wise in above-mentioned solution under standing or whipped state with 0.75～2mL tetraethoxy (TEOS), again under agitation, 0.20～0.94mL, 1mol/L europium nitrate solution and 0.20～1.00mL, 1mol/L Gadolinium trinitrate solution are joined respectively fast in the solution of step (1) (rare earth gadolinium, europium are mixed altogether);
(3) mixing solutions step (2) being obtained is water-bath 1～24h at 30 DEG C～80 DEG C, ethanol centrifuge washing final vacuum is dry, at 450 DEG C～650 DEG C, calcine 1～3h again, temperature rise rate is 5～8 DEG C/min, thereby obtains europium, the gadolinium codoped silica nanometer luminescent material of one-dimensional rod-like structure.
The method that the present invention adopts sol-gel synthesis to combine with calcination process, successfully prepares europium, the gadolinium codoped one dimension SiO of Rod-like shape
2nano material.Research shows that between rare earth ion, existing energy transfer process, its mechanism to be mainly eelctric dipole-eelctric dipole interacts, and is the result of non-radiative resonance absorption.When the volumetric molar concentration of rare earth ion list doping is respectively 10%Eu
3+, 9%Gd
3+time, it is the highest that intensity of emission spectra reaches; Along with Eu
3+, Gd
3+the increase of singly mixing concentration, luminous intensity is successively decreased gradually, and concentration quenching effect occurs.The ruddiness that prepared one dimension silicon dioxide nano rod nano luminescent material sends belongs to Eu
3+ion
5d
0-
7f
2transition, and Gd
3+at 314nm place corresponding to
6p
7/2→
8s
7/2the sharp line transmitting of transition, SiO
2: Eu
3+luminous have good monochromaticity.The inventive method workable, reaction conditions gentleness, favorable reproducibility, the feature that structure of title compound stable product homogeneity is good, and in silica matrix environment, realize rare earth Eu
3+, Gd
3+successful doping, and bring into play the high-quality characteristic of its luminous aspect, be a kind of effective ways of preparing monodimension nano stick luminescent material.
Brief description of the drawings
Fig. 1: 40 DEG C, stir and add reagent (NH
4oH, TEOS) the SEM figure (SiO of the europium of lower preparation, the silicon dioxide nano rod of gadolinium codoped
2: 9%Gd
3+, 10%Eu
3+); (the Eu calculating according to tetraethoxy stoichiometry
3+, Gd
3+doping volumetric molar concentration)
Fig. 2: 40 DEG C, stir and add reagent (NH
4oH, TEOS) the TEM figure (SiO of the europium of lower preparation, the silicon dioxide nano rod of gadolinium codoped
2: 9%Gd
3+, 10%Eu
3+);
Fig. 3: 40 DEG C, stir and add reagent (NH
4oH, TEOS) emmission spectrum (SiO of silicon dioxide nano rod of europium list doping of lower preparation
2: 10%Eu
3+, 393nm excites);
Fig. 4: 40 DEG C, stir and add reagent (NH
4oH, TEOS) emmission spectrum (SiO of silicon dioxide nano rod of gadolinium list doping of lower preparation
2: 9%Gd
3+, 274nm excites);
Fig. 5: 40 DEG C, stir and add reagent (NH
4oH, TEOS) the lower Eu preparing
3+singly mix excitation spectrum (1) and the Gd of silicon dioxide nano rod
3+emmission spectrum (the 2) (SiO of the silicon dioxide nano rod of singly mixing
2: 10%Eu
3+, 612nm transmitting; SiO
2: 9%Gd
3+, 274nm excites);
Fig. 6: 40 DEG C, stir and add reagent (NH
4oH, TEOS) europium of lower preparation, the silicon dioxide nano rod emmission spectrum (SiO of gadolinium codoped
2: 9%Gd
3+, y Eu
3+) (274nm excites);
Fig. 7: Eu
3+and Gd
3+energy level schematic diagram and energy transfer process schematic diagram;
Fig. 8: 40 DEG C, leave standstill and add reagent (NH
4oH, TEOS) the SEM figure (SiO of the europium of lower preparation, the silicon dioxide nano rod of gadolinium codoped
2: 9%Gd
3+, 10%Eu
3+);
Fig. 9: 30 DEG C, stir and add reagent (NH
4oH, TEOS) the SEM figure (SiO of the europium of lower preparation, the silicon dioxide nano rod of gadolinium codoped
2: 9%Gd
3+, 10%Eu
3+);
Figure 10,60 DEG C, stir and add reagent (NH
4oH, TEOS) the SEM figure (SiO of the europium of lower preparation, the silicon dioxide nano rod of gadolinium codoped
2: 9%Gd
3+, 10%Eu
3+);
Figure 11: 80 DEG C, stir and add reagent (NH
4oH, TEOS) the SEM figure (SiO of the europium of lower preparation, the silicon dioxide nano rod of gadolinium codoped
2: 9%Gd
3+, 10%Eu
3+);
Embodiment
Embodiment 1:
(1) 0.31g tensio-active agent cetyl trimethylammonium bromide (CTAB) and 0.05g dispersion agent polyoxyethylene glycol (PEG-2000) are dissolved in 50mL deionized water, and are positioned over and in 40 DEG C of water-baths, are stirred to tensio-active agent and dissolve completely;
(2) by 2mL ammoniacal liquor (NH
4oH) under whipped state, be slowly added drop-wise in above-mentioned solution with 1.5mL tetraethoxy (TEOS), again under agitation, by different mole doping contents as 3%, 7%, 10%, 12%, 14% by corresponding volume number be respectively 0.20,0.47,0.67,0.80, to join fast (rare-earth europium ion list is mixed) in above-mentioned mixing solutions be solution I～V to (1mol/L) europium nitrate solution of 0.94mL, determines the solution M (being the solution that europium ion mole doping content is 10%) of optimum molar doping content by spectrum;
(3) on the basis of (1), by 2mL ammoniacal liquor (NH
4oH) under whipped state, be slowly added drop-wise in above-mentioned solution with 1.5mL tetraethoxy (TEOS), again under agitation, be 10% by mole doping content, volume number be the europium nitrate solution of 0.67mL (1mol/L) and different mole doping contents as 3%, 7%, 9%, 12%, 15% by corresponding volume number be respectively 0.20,0.47,0.60,0.80, to join fast respectively (rare earth gadolinium europium is mixed altogether) in above-mentioned mixing solutions be solution VI～X to (1mol/L) Gadolinium trinitrate solution of 1.0mL;
(4) by above-mentioned mixing solutions M, VI～X leaves standstill 2h under 40 DEG C of water-baths, and ethanol centrifuge washing final vacuum is dry, then calcines 1h at 600 DEG C, temperature rise rate is 5 DEG C/min, thereby obtains the europium list doping of one-dimensional rod-like structure and europium, gadolinium codoped silicon dioxide nano rod structure.
Fig. 1 and Fig. 2 are given in scanning and the transmission electron microscope picture of the codoped silicon dioxide nano rod of preparation at 40 DEG C.As can be seen from the figure, it is good that the Rod-like shape of sample keeps, and length and the diameter of rod are about respectively 500～700nm and 200～300nm, and nanometer rod has smooth surface and good dispersiveness uniformly.
Fig. 3 has shown the emmission spectrum of the sample of the single europium doped making under different levels of doping, excitation wavelength 393nm.As seen from the figure, different Eu
3+the SiO of doping content
2the luminous intensity difference of nanometer rod, its variation tendency embodies concentration quenching principle.In the time that doping content rises to 14% gradually by 3%, along with Eu
3+the increase of concentration, luminous intensity is grow gradually, reaches maximum intensity 10% time; Along with Eu
3+concentration continues to increase, and luminous intensity weakens gradually, and this phenomenon has well embodied the concentration quenching effect of rare earth ion in the middle of matrix.Under 393nm excitation wavelength, emmission spectrum comprises
5d
0-
7f
j(J=0,1,2,3,4) (577,590,612,652, and 702nm) Eu
3+feature transition.The strongest emission peak is at 612nm place,
5d
0→
7f
2belong to electric dipole transition and mainly depend on a kind of symmetric position.
Fig. 4 is the emmission spectrum of single gadolinium-doped of making sample under different levels of doping, excitation wavelength 274nm.In the time that doping content is increased to 15% by 3%, along with Gd
3+the increase of concentration, luminous intensity presents the trend weakening after enhancing, reaches maximum intensity 9% time, and concentration quenching effect has occurred.Gd
3+there is a sharp line transmitting at 314nm place, corresponding to
6p
7/2→
8s
7/2transition.
Fig. 5 is Eu
3+excitation spectrum (a) and Gd
3+emmission spectrum (b) (a: λ
em=612nm, b: λ
ex=274nm).Eu as seen from the figure
3+excitation spectrum and Gd
3+emmission spectrum there is the condition of the overlapping Dexter of meeting transmission ofenergy, there is the possibility of transmission ofenergy.
Fig. 6 is the silicon dioxide nano rod emmission spectrum of europium, gadolinium codoped, fixing Gd
3+ionic concn changes Eu
3+ionic concn.As seen from the figure, along with Eu
3+the increase of concentration, Gd
3+emission peak weaken gradually, Eu
3+characteristic emission peak strengthen gradually, work as Eu
3+concentration reach maximum value while reaching 10% left and right, Gd can be described by above experimental result
3+→ Eu
3+there is effective transmission ofenergy.Continue to increase Eu
3+concentration, in the time that concentration reaches 10%, due to Eu
3+self concentration quenching make on the contrary luminous intensity decline, proving again the possibility of transmission ofenergy.
Fig. 7 is Eu
3+and Gd
3+energy level schematic diagram and energy transfer process.Gd
3+excited state and Ground State Energy differential be 32100cm
-1, with Eu
3+'s
5h
jexcited level matches.Under the exciting of 274nm UV-light, Gd
3+4f electronics from
8s
7/2ground state transition is arrived
6i
jexcited state then lattice relaxation arrives
6p
jexcited state, to resonate, excitation energy is passed to Eu by the mode of transmitting
3+'s
5h
jexcited state, and quick radiationless transition is extremely
5d
0energy level, warp
5d
0energy level transition is got back to 7F energy level and is occurred Eu
3+the transmitting of the sharp line of f-f.
Embodiment 2:
0.31g CTAB and 0.05g PEG-2000 are dissolved in deionized water, and are positioned in 40 DEG C of water-baths, to be stirred to completely and dissolve.Subsequently, under standing state, dropwise add 2mL NH
4oH and 1.5mL TEOS.Continuing is 10% by mole doping content, volume number be the europium nitrate solution of 0.67mL (1mol/L) and difference mole doping contents as 3%, 7%, 9%, 12%, 15% by corresponding volume number be respectively 0.20,0.47,0.60, (1mol/L) Gadolinium trinitrate solution of 1.0mL joins in above-mentioned mixing solutions under whipped state.Mixing solutions is left standstill after 2h, and ethanol centrifuge washing final vacuum is dry, then calcines 1h at 600 DEG C, and temperature rise rate is 5 DEG C/min.After having calcined, the sample obtaining is nanorod structure.
What Fig. 8 provided is under the condition of 40 DEG C, is leaving standstill interpolation reagent (NH
4oH, TEOS) Eu under condition
3+, Gd
3+the SiO of codoped
2the scanning electron microscope picture of nanometer rod.Compared to Figure 1, there is unequal distortion in nanometer rod, and length and diameter are about respectively 1-1.4 μ m and 200-300nm.Diameter does not roughly change, and length reaches micron order and is distorted, and this is due to leaving standstill under interpolation reagent condition, contributes to template micella to one-dimensional square to growth.
Embodiment 3:
The CTAB of 0.31g and 0.05g PEG-2000 are dissolved in deionized water, and are positioned in 40 DEG C of water-baths, to be stirred to completely and dissolve.Subsequently, by 2mL NH
4oH and 1.5mLTEOS are slowly added drop-wise in solution under vigorous stirring.Continuing is 10% by mole doping content, volume number be the europium nitrate solution of 0.67mL (1mol/L) and difference mole doping contents as 3%, 7%, 9%, 12%, 15% by corresponding volume number be respectively 0.20,0.47,0.60, (1mol/L) Gadolinium trinitrate solution of 1.0mL joins in above-mentioned mixing solutions under whipped state.Mixing solutions is left standstill after 2h, and ethanol centrifuge washing final vacuum is dry, then calcines 1h at 600 DEG C, and temperature rise rate is 5 DEG C/min.After having calcined, the sample obtaining is nanorod structure
What Fig. 9～11 provided is bath temperature (step 4) under the condition of 30 DEG C, 60 DEG C and 80 DEG C by 10%Eu
3+, 9%Gd
3+the SiO of codoped
2the scanning electron microscope picture of nanometer rod.Comparing Fig. 1 can find out, temperature is very large on the impact of pattern.In the time that temperature is lower, moment nucleation number less, precursor concentration raise, size heterogeneity; In the time that temperature is higher, precursor concentration reduce, moment nucleation number more, size reduce, length and diameter are about respectively 70nm～100nm and 50nm～80nm.And easily reunite.
Claims (4)
1. the SiO of an one-dimentional structure
2: Eu
3+, Gd
3+the preparation method of nano luminescent material, its step is as follows:
(1) tensio-active agent cetyl trimethylammonium bromide and dispersion agent polyoxyethylene glycol are dissolved in deionized water, and under 30 DEG C～80 DEG C water-baths, are stirred to tensio-active agent and dissolve completely;
(2) ammoniacal liquor and tetraethoxy are slowly added drop-wise in step (1) solution under standing or whipped state, more under agitation, europium nitrate solution and Gadolinium trinitrate solution are joined respectively in the solution of step (1) fast;
(3) mixing solutions step (2) being obtained is water-bath 1～24h at 30 DEG C～80 DEG C, ethanol centrifuge washing final vacuum is dry, at 450 DEG C～650 DEG C, calcine 1～3h again, thereby obtain europium, the gadolinium codoped silica nanometer luminescent material of one-dimensional rod-like structure.
2. the SiO of a kind of one-dimentional structure as claimed in claim 1
2: Eu
3+, Gd
3+the preparation method of nano luminescent material, is characterized in that: in step (1), be that 0.20～0.35g tensio-active agent cetyl trimethylammonium bromide and 0.03～0.07g dispersion agent polyoxyethylene glycol are dissolved in 30～70mL deionized water.
3. the SiO of a kind of one-dimentional structure as claimed in claim 1
2: Eu
3+, Gd
3+the preparation method of nano luminescent material, is characterized in that: in step (2), be that 1～3mL ammoniacal liquor and 0.75～2mL tetraethoxy are slowly added drop-wise in step (1) solution under standing or whipped state; Again under agitation, 0.20～0.94mL, 1mol/L europium nitrate solution and 0.20～1.00mL, 1mol/L Gadolinium trinitrate solution are joined respectively in the solution of step (1) fast.
4. the SiO of a kind of one-dimentional structure as claimed in claim 1
2: Eu
3+, Gd
3+the preparation method of nano luminescent material, is characterized in that: in step (3), the temperature rise rate of calcining is 5～8 DEG C/min.
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Cited By (2)
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|---|---|---|---|---|
| CN108380199A (en) * | 2018-03-16 | 2018-08-10 | 沈阳理工大学 | A method of preparing europium-titanium composite nano oxide powder |
| CN110713350A (en) * | 2019-10-22 | 2020-01-21 | 同济大学 | Preparation method of one-dimensional nano silicon dioxide |
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| CN101857237A (en) * | 2010-06-11 | 2010-10-13 | 济南大学 | Method for preparing mesoporous silicon dioxide nano rod through regulation and control |
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2014
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| CN101857237A (en) * | 2010-06-11 | 2010-10-13 | 济南大学 | Method for preparing mesoporous silicon dioxide nano rod through regulation and control |
Non-Patent Citations (2)
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| CHUNMING LIN ET AL: "Synthesis and luminescence properties of Eu(III)-doped silica nanorods based on the sol–gel process", 《JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380199A (en) * | 2018-03-16 | 2018-08-10 | 沈阳理工大学 | A method of preparing europium-titanium composite nano oxide powder |
| CN108380199B (en) * | 2018-03-16 | 2020-09-01 | 沈阳理工大学 | Method for preparing europium-titanium composite nano oxide powder |
| CN110713350A (en) * | 2019-10-22 | 2020-01-21 | 同济大学 | Preparation method of one-dimensional nano silicon dioxide |
| CN110713350B (en) * | 2019-10-22 | 2021-05-11 | 同济大学 | Preparation method of one-dimensional nano silicon dioxide |
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