CN103351859B - Method for preparing Ag/Y2O3:Yb<3+>/Er<3+> composite nanotubes with up-conversion light emitting function - Google Patents
Method for preparing Ag/Y2O3:Yb<3+>/Er<3+> composite nanotubes with up-conversion light emitting function Download PDFInfo
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Abstract
The invention discloses a method for preparing Ag/Y2O3:Yb<3+>/Er<3+> composite nanotubes with an up-conversion light emitting function, relating to a preparation method of composite nanotubes. The method is used for solving the technical problem of the existing rare-earth up-conversion fluorescent materials that the light emitting efficiency is low. The method comprises the following steps of: (1) adding a surfactant into a rare-earth solution, and adjusting the pH value; (2) carrying out heat treatment; (3) washing and drying so as to obtain Y(OH)3:Yb<3+>/Er<3+> nanotubes; and (4) mixing the Y(OH)3:Yb<3+>/Er<3+> nanotubes with a silver chloride solution through a depressurizing method, thoroughly stirring, drying and roasting, thereby preparing the Ag/Y2O3:Yb<3+>/Er<3+> composite nanotubes. The Ag/Y2O3:Yb<3+>/Er<3+> composite nanotubes prepared by the method are uniform in morphology, can emit green up-conversion fluorescent light and are high in light emitting efficiency. The method belongs to the field of preparation of composite nanotubes.
Description
Technical field
The present invention relates to a kind of preparation method of composite nano tube.
Background technology
The special electronic configuration of rare earth element makes it have special optical, electrical, magnetic property, and is described as the treasure-house of novel material.After rare earth nano, show numerous characteristics, as small-size effect, high-ratio surface effect, quantum effect, extremely strong optical, electrical, magnetic property, supraconductivity, high chemically reactive etc., can greatly improve performance and the function of material.The reported first such as Bhargava in 1994 nanometer ZnS: Mn there is very high fluorescence efficiency, people have caused great interest to semi-conductor nano luminescent material, because it has indicated that nano luminescent material may have the characteristics such as high luminous efficiency and short fluorescence lifetime.At present, rare earth mixing with nano fluorescent material has obtained research widely.Quantity research shows greatly, and rare earth nano material has broad application prospects in a lot of fields such as biology, medical treatment, catalysis, battery.Particularly the synthetic and application of rare-earth nanometer compound material has caused the extensive concern of Chinese scholars.For example, Qian Yitai seminar has synthesized Fe
3o
4/ NaYF
4: Nd
3+composite Double function nano material.The flat seminar of Qin Wei has synthesized TiO
2/ NaYF
4: Tm
3+/ Yb
3+nucleocapsid structure, has realized infrared light catalysis.
Precious metal was just paid close attention to by people before more than 2000 years, was applied in glass industry.In recent years, due to plasma resonance character and himself good bio-compatibility on noble metal nano particles surface, another becomes the focus of researcher research.People combine noble metal nano particles with function nano particle, successfully prepare and much have difunctional even multifunctional nano material, and be applied to multiple fields such as optics, biomedicine and therapeutics.The study group that is devoted at present this type of work has a lot.And existing rare earth upconverting fluorescent material luminous efficiency is low.
Summary of the invention
The object of the invention is, in order to solve the low technical problem of existing rare earth upconverting fluorescent material luminous efficiency, provides a kind of Ag/Y with up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube.
There is the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube carries out according to following steps:
One, be that 40～90 DEG C, stirring velocity are under 100～350 revs/min of conditions in temperature, concentration is to add tensio-active agent in the earth solution of 0.1～2mol/L, the mol ratio of earth solution and tensio-active agent is 1:1～10, and regulating pH value with ammonia soln is 14, stirs 20 minutes～24 hours;
Two, adopt solvent-thermal method to heat-treat the resultant through step 1;
Three, be 7 by product to the pH value of washing lotion of distilled water wash step 2, then vacuum-drying 3～24 hours under 60～80 DEG C of conditions, obtains Y (OH)
3: Yb
3+/ Er
3+nanotube;
Four, by decompression method by Y (OH)
3: Yb
3+/ Er
3+the silver chloride solution that is 0.1～2mol/L with concentration mixes, wherein Y (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.0001～0.1, stir, vacuum-drying 3～24 hours;
Five, be to rise to 400～700 DEG C under the condition of 1～20 DEG C/min at heat-up rate by the resultant of step 4, then, 400～700 DEG C of roastings 5 minutes～8 hours, obtain Ag/Y
2o
3: Yb
3+/ Er
3+composite nano tube.
Earth solution described in step 1 is rare earth nitrate solution.
Described rare earth nitrate solution is the mixing solutions of Yttrium trinitrate, ytterbium nitrate and Erbium trinitrate, and in mixing solutions, the concentration of Yttrium trinitrate is that the concentration of 0.1～2mol/L, ytterbium nitrate is that 0.1～2mol/L and Erbium trinitrate concentration are 0.1～2mol/L.
Tensio-active agent described in step 1 is sodium lauryl sulphate.
Solvent-thermal method described in step 2 is as follows:
The resultant of step 1 is dissolved in solvent, is thermal treatment 10～48 hours under the condition of 120 DEG C in temperature, and described solvent is the mixture of mixture, water and ethylene glycol or the mixture of ethanol and ethylene glycol of water, ethanol, ethylene glycol, water and ethanol.
Ag/Y prepared by the present invention
2o
3: Yb
3+/ Er
3+composite nano tube, Ag nano-crystalline granule is compound to Y
2o
3: Yb
3+/ Er
3+on nanotube, and the Ag/Y of preparation
2o
3: Yb
3+/ Er
3+composite nano tube pattern homogeneous, can send green up-conversion fluorescence, luminous efficiency is high; Present method technique is simple, cost is low, required equipment is simple, production security is strong, is easy to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the Ag/Y with up-conversion luminescence function of experiment one preparation
2o
3: Yb
3+/ Er
3+the electron scanning micrograph of composite nano tube;
Fig. 2 is the Ag/Y with up-conversion luminescence function of experiment one preparation
2o
3: Yb
3+/ Er
3+the XRD spectra of composite nano tube;
Fig. 3 is the Ag/Y with up-conversion luminescence function of experiment one preparation
2o
3: Yb
3+/ Er
3+the upper switching emission spectrum of composite nano tube.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment has the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube carries out according to following steps:
One, be that 40～90 DEG C, stirring velocity are under 100～350 revs/min of conditions in temperature, concentration is to add tensio-active agent in the earth solution of 0.1～2mol/L, the mol ratio of earth solution and tensio-active agent is 1:1～10, and regulating pH value with ammonia soln is 14, stirs 20 minutes～24 hours;
Two, adopt solvent-thermal method to heat-treat the resultant through step 1;
Three, be 7 by product to the pH value of washing lotion of distilled water wash step 2, then vacuum-drying 3～24 hours under 60～80 DEG C of conditions, obtains Y (OH)
3: Yb
3+/ Er
3+nanotube;
Four, by decompression method by Y (OH)
3: Yb
3+/ Er
3+the silver chloride solution that is 0.1～2mol/L with concentration mixes, wherein Y (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.0001～0.1, stir, vacuum-drying 3～24 hours;
Five, be to rise to 400～700 DEG C under the condition of 1～20 DEG C/min at heat-up rate by the resultant of step 4, then, 400～700 DEG C of roastings 5 minutes～8 hours, obtain Ag/Y
2o
3: Yb
3+/ Er
3+composite nano tube.
Embodiment two: what present embodiment was different from embodiment one is that the earth solution described in step 1 is rare earth nitrate solution.Other is identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment two is that described rare earth nitrate solution is the mixing solutions of Yttrium trinitrate, ytterbium nitrate and Erbium trinitrate, in mixing solutions, the concentration of Yttrium trinitrate is that the concentration of 0.1～2mol/L, ytterbium nitrate is that 0.1～2mol/L and Erbium trinitrate concentration are 0.1～2mol/L.Other is not identical with embodiment two.
Embodiment four: the tensio-active agent described in step 1 that what present embodiment was different from one of embodiment one to three is is sodium lauryl sulphate.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different from one of embodiment one to four is that the solvent-thermal method described in step 2 is as follows:
The resultant of step 1 is dissolved in solvent, is thermal treatment 10～48 hours under the condition of 120 DEG C in temperature, and described solvent is the mixture of mixture, water and ethylene glycol or the mixture of ethanol and ethylene glycol of water, ethanol, ethylene glycol, water and ethanol.Other is identical with one of embodiment one to four.
When solvent described in present embodiment is mixture, between each composition, be arbitrarily than.
Embodiment six: the method for decompression described in step 4 that what present embodiment was different from one of embodiment one to five is is to be that 15～40 DEG C, the relative vacuum degree of pressure are by Y (OH) under 0～-0.2MPa condition in temperature
3: Yb
3+/ Er
3+with concentration be 0.1～2mol/L silver chloride solution mix 0.2～4h.Other is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is in step 1 in temperature is that 50 DEG C, stirring velocity are under 200 revs/min of conditions, adds tensio-active agent in the earth solution that concentration is 0.5mol/L.Other is identical with one of embodiment one to six.
Embodiment eight: the mol ratio of what present embodiment was different from one of embodiment one to seven is step 1 middle-weight rare earths solution and tensio-active agent is 1:5.Other is identical with one of embodiment one to seven.
Embodiment nine: that present embodiment is different from one of embodiment one to eight is Y in step 4 (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.01.Other is identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different from one of embodiment one to nine is is to rise to 500 DEG C under the condition of 15 DEG C/min at heat-up rate by the resultant of step 4 in step 5, then 500 DEG C of roastings 5 hours.Other is identical with one of embodiment one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
There is the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube carries out according to following steps:
One, be that 90 DEG C, stirring velocity are under 350 revs/min of conditions in temperature, concentration is to add sodium lauryl sulphate in the earth solution of 2mol/L, the mol ratio of earth solution and sodium lauryl sulphate is 1:10, and regulating pH value with ammonia soln is 14, stirs 24 hours;
Two, adopt solvent-thermal method to heat-treat the resultant through step 1;
Three, be 7 by product to the pH value of washing lotion of distilled water wash step 2, then vacuum-drying 12 hours under 60 DEG C of conditions, obtains Y (OH)
3: Yb
3+/ Er
3+nanotube;
Four, by decompression method by Y (OH)
3: Yb
3+/ Er
3+the silver chloride solution that is 2mol/L with concentration mixes, wherein Y (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.1, stir, vacuum-drying 12 hours, the method for decompression described in step 4 be temperature be 20 DEG C, the relative vacuum degree of pressure under-0.1MPa condition by Y (OH)
3: Yb
3+/ Er
3+with concentration be 1.5mol/L silver chloride solution mixing 2h;
Five, be to rise to 600 DEG C under the condition of 20 DEG C/min at heat-up rate by the resultant of step 4, then, 600 DEG C of roastings 8 hours, obtain Ag/Y
2o
3: Yb
3+/ Er
3+composite nano tube.
As can be seen from Figure 1, composite nano tube pattern homogeneous.Fig. 2 is Ag/Y for this reason
2o
3: Yb
3+/ Er
3+the XRD spectra of composite nano tube, the as can be seen from the figure Ag of cube crystalline phase and Y
2o
3: Yb
3+/ Er
3+coexist.Fig. 3 is Ag/Y for this reason
2o
3: Yb
3+/ Er
3+the upper switching emission spectrum of composite nano tube, as can be seen from the figure sample can send green up-conversion fluorescence.
Experiment two:
There is the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube carries out according to following steps:
One, be that 40 DEG C, stirring velocity are under 100 revs/min of conditions in temperature, in the earth solution that concentration is 0.1mol/L, add tensio-active agent, the mol ratio of earth solution and tensio-active agent is 1:1, and regulating pH value with ammonia soln is 14, stirs 20 minutes;
Two, adopt solvent-thermal method to heat-treat the resultant through step 1;
Three, be 7 by product to the pH value of washing lotion of distilled water wash step 2, then vacuum-drying 3 hours under 60 DEG C of conditions, obtains Y (OH)
3: Yb
3+/ Er
3+nanotube;
Four, by decompression method by Y (OH)
3: Yb
3+/ Er
3+the silver chloride solution that is 0.1mol/L with concentration mixes, wherein Y (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.0001, stir, decompression method described in 3～24 hours step 4 of vacuum-drying is to be that 15 DEG C, the relative vacuum degree of pressure are by Y (OH) under 0MPa condition in temperature
3: Yb
3+/ Er
3+with concentration be 0.1mol/L silver chloride solution mixing 0.2h;
Five, be to rise to 400 DEG C under the condition of 1 DEG C/min at heat-up rate by the resultant of step 4, then, 400 DEG C of roastings 5 minutes, obtain Ag/Y
2o
3: Yb
3+/ Er
3+composite nano tube.
Experiment three:
There is the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube carries out according to following steps:
One, be that 90 DEG C, stirring velocity are under 350 revs/min of conditions in temperature, in the earth solution that concentration is 2mol/L, add tensio-active agent, the mol ratio of earth solution and tensio-active agent is 1:10, and regulating pH value with ammonia soln is 14, stirs 24 hours;
Two, adopt solvent-thermal method to heat-treat the resultant through step 1;
Three, be 7 by product to the pH value of washing lotion of distilled water wash step 2, then vacuum-drying 3～24 hours under 80 DEG C of conditions, obtains Y (OH)
3: Yb
3+/ Er
3+nanotube;
Four, by decompression method by Y (OH)
3: Yb
3+/ Er
3+the silver chloride solution that is 2mol/L with concentration mixes, wherein Y (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.001, stir, decompression method described in 20 hours step 4 of vacuum-drying be temperature be 40 DEG C, the relative vacuum degree of pressure under-0.2MPa condition by Y (OH)
3: Yb
3+/ Er
3+with concentration be 2mol/L silver chloride solution mixing 4h;
Five, be to rise to 500 DEG C under the condition of 15 DEG C/min at heat-up rate by the resultant of step 4, then, 500 DEG C of roastings 3 hours, obtain Ag/Y
2o
3: Yb
3+/ Er
3+composite nano tube.
Claims (8)
1. there is the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, is characterized in that having the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube carries out according to following steps:
One, be that 40～90 DEG C, stirring velocity are under 100～350 revs/min of conditions in temperature, concentration is to add tensio-active agent in the earth solution of 0.1～2mol/L, the mol ratio of earth solution and tensio-active agent is 1:1～10, and regulating pH value with ammonia soln is 14, stirs 20 minutes～24 hours;
Two, adopt solvent-thermal method to heat-treat the resultant through step 1;
Three, be 7 by product to the pH value of washing lotion of distilled water wash step 2, then vacuum-drying 3-24 hour under 60～80 DEG C of conditions, obtains Y (OH)
3: Yb
3+/ Er
3+nanotube;
Four, by decompression method by Y (OH)
3: Yb
3+/ Er
3+the silver chloride solution that is 0.1～2mol/L with concentration mixes, wherein Y (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.0001～0.1, stir, vacuum-drying 3-24 hour;
Five, be to rise to 400～700 DEG C under the condition of 1～20 DEG C/min at heat-up rate by the resultant of step 4, then, 400～700 DEG C of roastings 5 minutes～8 hours, obtain Ag/Y
2o
3: Yb
3+/ Er
3+composite nano tube;
Tensio-active agent described in step 1 is sodium lauryl sulphate;
Solvent-thermal method described in step 2 is as follows:
The resultant of step 1 is dissolved in solvent, is thermal treatment 10～48 hours under the condition of 120 DEG C in temperature, and described solvent is the mixture of mixture, water and ethylene glycol or the mixture of ethanol and ethylene glycol of water, ethanol, ethylene glycol, water and ethanol.
2. there is according to claim 1 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, is characterized in that the earth solution described in step 1 is rare earth nitrate solution.
3. there is according to claim 2 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, it is characterized in that described rare earth nitrate solution is the mixing solutions of Yttrium trinitrate, ytterbium nitrate and Erbium trinitrate, in mixing solutions, the concentration of Yttrium trinitrate is that the concentration of 0.1～2mol/L, ytterbium nitrate is that 0.1～2mol/L and Erbium trinitrate concentration are 0.1～2mol/L.
4. there is according to claim 1 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, is characterized in that the method for decompression described in step 4 is is that 15～40 DEG C, the relative vacuum degree of pressure are by Y (OH) under 0～-0.2MPa condition in temperature
3: Yb
3+/ Er
3+with concentration be 0.1～2mol/L silver chloride solution mix 0.2～4h.
5. there is according to claim 1 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, is characterized in that in step 1 in temperature being that 50 DEG C, stirring velocity are under 200 revs/min of conditions, in the earth solution that concentration is 0.5mol/L, adds tensio-active agent.
6. there is according to claim 1 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, the mol ratio that it is characterized in that step 1 middle-weight rare earths solution and tensio-active agent is 1:5.
7. there is according to claim 1 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, is characterized in that Y in step 4 (OH)
3: Yb
3+/ Er
3+with the mass ratio of silver chloride be 1:0.01.
8. there is according to claim 1 the Ag/Y of up-conversion luminescence function
2o
3: Yb
3+/ Er
3+the preparation method of composite nano tube, is characterized in that in step 5 being to rise to 500 DEG C under the condition of 15 DEG C/min at heat-up rate by the resultant of step 4, then 500 DEG C of roastings 5 hours.
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| CN105776308B (en) * | 2016-04-08 | 2017-11-21 | 天津城建大学 | It is a kind of using rare-earth oxidation yttrium nanotube as micron spheroid of primitive and preparation method thereof |
| CN106544020B (en) * | 2016-09-23 | 2019-03-22 | 长安大学 | The rear-earth-doped tungstate luminescent material and preparation method of nano-Ag particles enhancing |
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