CN104774616A - Preparation method of Y2O3/Y2O2S: Er<3+ > composite nanorod - Google Patents
Preparation method of Y2O3/Y2O2S: Er<3+ > composite nanorod Download PDFInfo
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- CN104774616A CN104774616A CN201510187548.6A CN201510187548A CN104774616A CN 104774616 A CN104774616 A CN 104774616A CN 201510187548 A CN201510187548 A CN 201510187548A CN 104774616 A CN104774616 A CN 104774616A
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- composite nanorod
- nanorod
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Abstract
The invention discloses a preparation method of an Y2O3/Y2O2S: Er<3+> composite nanorod. The invention relates to a preparation method of an Y2O3/Y2O2S: Er<3+> composite nanorod, and aims to solve the problem that an oxide up-conversion luminescent material is weak in luminescence. The preparation method comprises the following specific steps: 1, adding sodium hydroxide into a mixed solution of yttrium nitrate and erbium nitrate, and stirring; 2, carrying out heat treatment on the obtained object; 3. washing, and drying the obtained object so as to obtain a Y(OH)3: Er<3+> nanorod; and 4, sufficiently mixing the Y(OH)3: Er<3+> nanorod with sulfur powder, and roasting the obtained mixture so as to obtain an Y2O3/Y2O2S: Er<3+> composite nanorod. The Y2O3/Y2O2S: Er<3+> composite nanorod prepared according to the invention is a good up-conversion luminescent material. The method disclosed by the invention is applied to the field of nanocomposite preparation.
Description
Technical field
The present invention relates to a kind of Y
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod.
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., greatly can improve performance and the function of material.Large quantity research shows, rare earth nano material has broad application prospects in a lot of field such as biology, medical treatment, catalysis, battery.But because oxide compound phonon energy is high, cause oxide compound to be that the luminous efficiency of the rare earth up-conversion luminescent material of matrix is very low, even luminous.
Summary of the invention
The object of the invention is, in order to solve the luminous weak problem of oxide compound up-conversion luminescent material, to provide a kind of Y
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod.
A kind of Y of the present invention
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, carries out: one, by the ratio mixing of yttrium nitrate aqueous solution and Erbium trinitrate aqueous solution 49:1 in mass ratio, add the NaOH solution that concentration is 0.5mol/L, continue to stir, obtain mixing solutions after stirring according to the following steps; Two, mixing solutions is heat-treated, then wash vacuum-drying again, obtain Y (OH)
3: Er
3+nanometer rod; Three, the Y (OH) step 2 obtained
3: Er
3+nanometer rod and sulphur powder 1:(0.1 ~ 2 in mass ratio) ratio mixing, under nitrogen protection, roasting 0.5 ~ 2h at temperature is 800 DEG C, obtains Y
2o
3/ Y
2o
2s:Er
3+composite nanorod, namely completes.
The present invention is by Y (OH)
3: Er
3+nanometer rod top layer is successfully sulfided into Y
2o
2s:Er
3+, obtain the Y with nucleocapsid structure
2o
3/ Y
2o
2s:Er
3+composite nanorod, the Y of preparation
2o
3/ Y
2o
2s:Er
3+composite nanorod is good up-conversion luminescent material.Technique prepared by the present invention is simple, cost is low, required equipment is simple, production security is strong, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is Y prepared by test 1
2o
3/ Y
2o
2s:Er
3+the transmission electron microscope photo of composite nanorod;
Fig. 2 is Y prepared by test 1
2o
3/ Y
2o
2s:Er
3+the XRD spectrum of composite nanorod;
Fig. 3 is Y prepared by test 1
2o
3/ Y
2o
2s:Er
3+the upconversion emission of composite nanorod.
Embodiment
Embodiment one: a kind of Y of present embodiment
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, carries out: one, by the ratio mixing of yttrium nitrate aqueous solution and Erbium trinitrate aqueous solution 49:1 in mass ratio, add the NaOH solution that concentration is 0.5mol/L, continue to stir, obtain mixing solutions after stirring according to the following steps; Two, mixing solutions is heat-treated, then wash vacuum-drying again, obtain Y (OH)
3: Er
3+nanometer rod; Three, the Y (OH) step 2 obtained
3: Er
3+nanometer rod and sulphur powder 1:(0.1 ~ 2 in mass ratio) ratio mixing, under nitrogen protection, roasting 0.5 ~ 2h at temperature is 800 DEG C, obtains Y
2o
3/ Y
2o
2s:Er
3+composite nanorod, namely completes.
Present embodiment is by Y (OH)
3: Er
3+nanometer rod top layer is successfully sulfided into Y
2o
2s:Er
3+, obtain the Y with nucleocapsid structure
2o
3/ Y
2o
2s:Er
3+composite nanorod, the Y of preparation
2o
3/ Y
2o
2s:Er
3+composite nanorod is good up-conversion luminescent material.Technique prepared by present embodiment is simple, cost is low, required equipment is simple, production security is strong, is easy to realize suitability for industrialized production.
Embodiment two: present embodiment and embodiment one unlike: the mass concentration of the yttrium nitrate aqueous solution described in step one is 0.5mol/L, and the mass concentration of the Erbium trinitrate aqueous solution is 0.5mol/L.Other are identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the ratio of yttrium nitrate aqueous solution and Erbium trinitrate aqueous solution 49:1 in mass ratio being mixed described in step one, adding concentration after stirring is that the NaOH solution of 0.5mol/L is to pH=12.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: add the NaOH solution that concentration is 0.5mol/L after the stirring described in step one, continue stir 1h.Other steps are identical with one of embodiment one to three with parameter.
Embodiment five: one of present embodiment and embodiment one to four unlike: the speed of the stirring described in step one is 100 revs/min.Other steps are identical with one of embodiment one to four with parameter.
Embodiment six: one of present embodiment and embodiment one to five unlike: the heat treated temperature described in step 2 is 180 DEG C, and the time is 10h.Other steps are identical with one of embodiment one to five with parameter.
Embodiment seven: one of present embodiment and embodiment one to six to refer to the mixing solutions washing after thermal treatment with distilled water to pH=7 unlike, the washing described in step 2.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike, the vacuum-drying described in step 2 is vacuum-drying 10h at 80 DEG C.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike, Y (OH) the 3:Er3+ nanometer rod that the step 2 described in step 3 obtains and the mass ratio of sulphur powder are 1:0.2.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine are 1 DEG C/min unlike the speed of the intensification described in step 3.Other is identical with one of embodiment one to nine.
By following verification experimental verification beneficial effect of the present invention:
Test 1: the preparation method of a kind of plant butter containing food fibre of this test test group, carry out according to the following steps:
One, be 20 DEG C in temperature, under stirring velocity is 100 revs/min of conditions, in the ratio mixing by yttrium nitrate aqueous solution and Erbium trinitrate aqueous solution 49:1 in mass ratio, adds the NaOH solution that concentration is 0.5mol/L after stirring, continue to stir 1h, obtain mixing solutions; Two, by mixing solutions at 180 DEG C of thermal treatment 10h, be then washed with distilled water to pH=7, then at 80 DEG C vacuum-drying 10h, obtain Y (OH)
3: Er
3+nanometer rod; Three, the Y (OH) step 3 obtained
3: Er
3+nanometer rod and sulphur powder mix according to the ratio of mass ratio 1:0.2, and under nitrogen protection, roasting 2h at temperature is 80 DEG C, obtains Y
2o
3/ Y
2o
2s:Er
3+composite nanorod.
The Y of this test preparation
2o
3/ Y
2o
2s:Er
3+the transmission electron microscope photo of composite nanorod as shown in Figure 1, as can be seen from Figure 1, Y
2o
3/ Y
2o
2s:Er
3+composite nano materials has Rod-like shape.Fig. 2 is the Y of this test preparation
2o
3/ Y
2o
2s:Er
3+the XRD spectrum of composite nanorod, as can be seen from the figure Y
2o
3: Er
3+and Y
2o
2s:Er
3+coexist.Fig. 3 is the Y of this test preparation
2o
3/ Y
2o
2s:Er
3+the upconversion emission of composite nanorod, as can be seen from the figure Y
2o
3/ Y
2o
2s:Er
3+composite nanorod is good up-conversion luminescent material.
By Y (OH)
3: Er
3+nanometer rod top layer is successfully sulfided into Y
2o
2s:Er
3+, obtain the Y with nucleocapsid structure
2o
3/ Y
2o
2s:Er
3+composite nanorod, the Y of preparation
2o
3/ Y
2o
2s:Er
3+composite nanorod is good up-conversion luminescent material.Technique prepared by present embodiment is simple, cost is low, required equipment is simple, production security is strong, is easy to realize suitability for industrialized production.
Claims (10)
1. a Y
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, it is characterized in that it carries out according to the following steps: one, by the ratio mixing of yttrium nitrate aqueous solution and Erbium trinitrate aqueous solution 49:1 in mass ratio, add the NaOH solution that concentration is 0.5mol/L after stirring, continue to stir, obtain mixing solutions; Two, mixing solutions is heat-treated, then wash vacuum-drying again, obtain Y (OH)
3: Er
3+nanometer rod; Three, the Y (OH) step 2 obtained
3: Er
3+nanometer rod and sulphur powder 1:(0.1 ~ 2 in mass ratio) ratio mixing, under nitrogen protection, be warming up to 800 DEG C, then roasting 0.5 ~ 2h, obtains Y
2o
3/ Y
2o
2s:Er
3+composite nanorod, namely completes.
2. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, is characterized in that the mass concentration of the yttrium nitrate aqueous solution described in step one is 0.5mol/L, and the mass concentration of the Erbium trinitrate aqueous solution is 0.5mol/L.
3. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, it is characterized in that described in step one by the ratio mixing of yttrium nitrate aqueous solution and Erbium trinitrate aqueous solution 49:1 in mass ratio, adding concentration after stirring is that the NaOH solution of 0.5mol/L is to pH=12.
4. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, adds the NaOH solution that concentration is 0.5mol/L after it is characterized in that the stirring described in step one, continue to stir 1h.
5. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, is characterized in that the speed of the stirring described in step one is 100 revs/min.
6. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, it is characterized in that the heat treated temperature described in step 2 is 180 DEG C, the time is 10h.
7. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, the washing that it is characterized in that described in step 2 to refer to the mixing solutions washing after thermal treatment with distilled water to pH=7.
8. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, is characterized in that the vacuum-drying described in step 2 is vacuum-drying 10h at 80 DEG C.
9. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, is characterized in that the Y (OH) that the step 2 described in step 3 obtains
3: Er
3+the mass ratio of nanometer rod and sulphur powder is 1:0.2.
10. a kind of Y according to claim 1
2o
3/ Y
2o
2s:Er
3+the preparation method of composite nanorod, is characterized in that the speed of the intensification described in step 3 is 1 DEG C/min.
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|---|---|---|---|
| CN201510187548.6A CN104774616B (en) | 2015-04-20 | 2015-04-20 | A kind of Y2o3/ Y2o2s:Er3+the preparation method of composite nanorod |
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|---|---|---|---|
| CN201510187548.6A CN104774616B (en) | 2015-04-20 | 2015-04-20 | A kind of Y2o3/ Y2o2s:Er3+the preparation method of composite nanorod |
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| CN104774616A true CN104774616A (en) | 2015-07-15 |
| CN104774616B CN104774616B (en) | 2016-08-24 |
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199734A (en) * | 2015-10-26 | 2015-12-30 | 黑龙江大学 | Preparation method of Y2O3/Y2O2S:Eu<3+> composite nanoparticles |
Citations (4)
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|---|---|---|---|---|
| JPS57151680A (en) * | 1981-03-16 | 1982-09-18 | Nec Corp | Yellowish green fluorescent substance excited with low- speed electron rays |
| EP0491406A1 (en) * | 1990-12-15 | 1992-06-24 | Samsung Display Devices Co., Ltd. | Red pigment coated phosphor and method for manufacturing the same |
| CN102392324A (en) * | 2011-08-30 | 2012-03-28 | 长春理工大学 | Method for preparing terbium-doped yttrium oxide sulfide green fluorescent nanometer belt |
| CN103524128A (en) * | 2013-10-12 | 2014-01-22 | 南昌大学 | Preparation method of yttria-stabilized zirconia tetragonal nano powder with high specific surface area |
-
2015
- 2015-04-20 CN CN201510187548.6A patent/CN104774616B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57151680A (en) * | 1981-03-16 | 1982-09-18 | Nec Corp | Yellowish green fluorescent substance excited with low- speed electron rays |
| EP0491406A1 (en) * | 1990-12-15 | 1992-06-24 | Samsung Display Devices Co., Ltd. | Red pigment coated phosphor and method for manufacturing the same |
| CN102392324A (en) * | 2011-08-30 | 2012-03-28 | 长春理工大学 | Method for preparing terbium-doped yttrium oxide sulfide green fluorescent nanometer belt |
| CN103524128A (en) * | 2013-10-12 | 2014-01-22 | 南昌大学 | Preparation method of yttria-stabilized zirconia tetragonal nano powder with high specific surface area |
Non-Patent Citations (3)
| Title |
|---|
| HAN PENGDE等: "Investigation on the amounts of Na2CO3 and sulphur to obtain pure Y2O2S and up-conversion luminescence of Y2O2S:Er", 《JOURNAL OF RARE EARTHS》, vol. 29, no. 9, 30 September 2011 (2011-09-30), pages 849 - 854 * |
| XUN WANG等: "Rare Earth Compound Nanotubes", 《ADVANCED MATERIALS》, vol. 15, no. 17, 3 September 2003 (2003-09-03), pages 1442 - 1445 * |
| 柏朝晖等: "Y2O2S：Er3+，Yb3+的制备及Er3+离子在晶场中的能级***", 《无机化学学报》, vol. 28, no. 4, 30 April 2012 (2012-04-30), pages 674 - 678 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199734A (en) * | 2015-10-26 | 2015-12-30 | 黑龙江大学 | Preparation method of Y2O3/Y2O2S:Eu<3+> composite nanoparticles |
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