CN103074061A - Synthetic method of rare earth nanometer nuclear shell spherical particle luminescent material - Google Patents
Synthetic method of rare earth nanometer nuclear shell spherical particle luminescent material Download PDFInfo
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- CN103074061A CN103074061A CN2013100016147A CN201310001614A CN103074061A CN 103074061 A CN103074061 A CN 103074061A CN 2013100016147 A CN2013100016147 A CN 2013100016147A CN 201310001614 A CN201310001614 A CN 201310001614A CN 103074061 A CN103074061 A CN 103074061A
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Abstract
The invention discloses a synthetic method of a rear earth nanometer nuclear shell spherical particle luminescent material, and relates to a synthetic method of a luminescent material. The Stober process is used for synthesizing a spherical SiO2 core as follows: dissolving TEOS (tetraethoxysilane) in an ethanol solution containing water and ammonia, stirring at the room temperature, centrifuging, keeping at the constant temperature for hours and drying; and the sol-gel process is used for synthesizing SiO2@Lu2O3:Ln<3+>(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particles with a core-shell structure as follows: dissolving lutetium oxide and oxide mixed with rare earth in nitric acid, mixing with a water-ethanol solution containing citric acid, adding PEG (polyethylene glycol), stirring, adding silicon particles, stirring, centrifuging a suspension liquid, precipitating, drying, and performing high temperature treatment to obtain products. The obtained products give out light in different colors respectively, have uniform shape and appearance, and are valuable luminescent materials.
Description
Technical field
The present invention relates to a kind of synthetic method of luminescent material, particularly relate to the synthetic method of the spherical particle light-emitting material of a kind of rare earth nano nucleocapsid.
Background technology
Rare earth is a huge mine of luminescent materials, and in the various luminescent materials of human development, rare earth element is being brought into play very important effect.Rare earth luminescent material once played a part milestone in the development of luminescence and luminescent material.Especially in recent years, the Study of Nanoscale Rare Earth Luminescent Materials that has a nucleocapsid structure pattern all has been subject to paying close attention to widely in catalysis, isolation technique, microelectronic device and biotechnology field.So far, people are making very large effort aspect the synthetic method of design different structure core-shell material and different shells.Even now, for utilize simple method just can realize having unified size, evenly still there is very large challenge the material aspect of the adjustable rare earth nano nucleocapsid structure of pattern and function.
Summary of the invention
The object of the present invention is to provide the synthetic method of the spherical particle light-emitting material of a kind of rare earth nano nucleocapsid.Present method utilizes a simple sol-gel process and high-temperature roasting afterwards just can obtain meeting the SiO of above-mentioned requirements
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle.This product has uniform pattern, is a kind of valuable luminescent material.
The objective of the invention is to be achieved through the following technical solutions:
The synthetic method of the spherical particle light-emitting material of a kind of rare earth nano nucleocapsid, described method comprises following process:
(1) closes glomerate SiO with St ber process
2Nuclear: by tetraethoxy (TEOS) is dissolved in the ethanolic soln that contains water and ammonia, stir under the room temperature, centrifugal, constant temperature a few hours oven dry;
(2) SiO by sol-gel process synthetic kernel shell structure
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle: the oxide compound of lutecium oxide and the rare earth that mixes is dissolved in nitric acid, then mix with the water-ethanol solution that contains citric acid, add polyoxyethylene glycol (PEG), then stir, add the silicon grain that obtains in (1), then stir, centrifugal to suspension afterwards, the precipitation oven dry, pyroprocessing obtains product.
The synthetic method of the spherical particle light-emitting material of described a kind of rare earth nano nucleocapsid, the described product that obtains is the SiO of nucleocapsid structure
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle.
Advantage of the present invention and effect are:
The present invention obtains by a simple sol-gel and pyroprocessing, and to have carried out different colours luminous by mixing different rare earth ions, by changing different rare earth ion Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) doping SiO
2Lu
2O
3Particle, resulting product presents respectively the luminous of different colours, and this product has uniform pattern, is a kind of valuable luminescent material.
Description of drawings
Fig. 1 is SiO
2Lu
2O
3: Eu
3+SEM and TEM, SiO
2Lu
2O
3: Ln
3+The coordinate of each luminous point of (Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) in colour light emitting coordinate CIE, the excitation spectrum of photoluminescence;
Fig. 2 is SiO
2Lu
2O
3: Eu
3+SEM and TEM, SiO
2Lu
2O
3: Ln
3+The coordinate of each luminous point in colour light emitting coordinate CIE of (Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm), the utilizing emitted light spectrogram of photoluminescence.
Annotate: Fig. 1-Fig. 2 of the present invention is analysis synoptic diagram or the photo (only for reference) of product state, the unintelligible understanding that does not affect technical solution of the present invention of figure Chinese word or image.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
The invention provides a kind of simple sol-gel process and pyroprocessing synthesize have unified size, the even SiO of pattern
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle.In addition, to different rare earth ion Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) doping SiO
2Lu
2O
3The luminosity of particle is studied.
The present invention closes glomerate SiO with St ber process
2Nuclear: by tetraethoxy (TEOS) is dissolved in the ethanolic soln that contains water and ammonia, stirred for several hour under the room temperature, centrifugal, constant temperature a few hours dry at a certain temperature.SiO by sol-gel process synthetic kernel shell structure
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle: the oxide compound of a certain amount of lutecium oxide and the rare earth that mixes is dissolved in nitric acid, then mixes with the water-ethanol solution that contains citric acid, adds certain density polyoxyethylene glycol (PEG).Then stirred for several hour adds the particle of the silicon that obtains in (1), then stirs, and is centrifugal to suspension afterwards, the precipitation oven dry.Process under the high temperature and obtain product.
Resulting product is the SiO of nucleocapsid structure
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle.It is a kind of valuable luminescent material.
Fig. 1 and Fig. 2 are respectively SiO
2Lu
2O
3: Eu
3+SEM and TEM, SiO
2Lu
2O
3: Ln
3+The coordinate of each luminous point of (Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) in colour light emitting coordinate CIE, excitation spectrum and the utilizing emitted light spectrogram of photoluminescence.
Embodiment:
(1) in ethanol (70-80 mL) solution of tetraethoxy (TEOS) (8-10 mL) water-soluble (15-20 mL) and ammonia (90-100 mL), stirred 3-5 hour under the room temperature, centrifugation is in the oven dry in 12 hours of 90-100 ℃ of lower constant temperature.
(2) oxide compound of lutecium oxide and the rare earth that mixes is dissolved in nitric acid, and then (V:V=1:7) solution mixes, and adds the polyoxyethylene glycol (PEG) of 0.10-0.20 g/mL with the water-ethanol that contains citric acid.Then stirred 4-6 hour, and added the particle of the silicon that obtains in (1), then stirred 12 hours, centrifugal to suspension afterwards, be deposited in the oven dry in 12 hours of 90-100 ℃ of lower constant temperature.Then with obtaining product in 700-900 ℃ of roasting 3-5 hour.
Claims (2)
1. the synthetic method of the spherical particle light-emitting material of rare earth nano nucleocapsid is characterized in that, described method comprises following process:
(1) closes glomerate SiO with St ber process
2Nuclear: by tetraethoxy (TEOS) is dissolved in the ethanolic soln that contains water and ammonia, stir under the room temperature, centrifugal, constant temperature a few hours oven dry;
(2) SiO by sol-gel process synthetic kernel shell structure
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle: the oxide compound of lutecium oxide and the rare earth that mixes is dissolved in nitric acid, then mix with the water-ethanol solution that contains citric acid, add polyoxyethylene glycol (PEG), then stir, add the silicon grain that obtains in (1), then stir, centrifugal to suspension afterwards, the precipitation oven dry, pyroprocessing obtains product.
2. the synthetic method of the spherical particle light-emitting material of a kind of rare earth nano nucleocapsid according to claim 1 is characterized in that the described product that obtains is the SiO of nucleocapsid structure
2Lu
2O
3: Ln
3+(Ln=Eu, Tb, Dy, Sm, Er, Ho and Tm) spherical particle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312558A (en) * | 2014-07-30 | 2016-02-10 | 苏州环球色谱有限责任公司 | Method for preparing core-shell type granules and application of core-shell type granules prepared with method |
| CN107619278A (en) * | 2017-10-25 | 2018-01-23 | 长春理工大学 | Double-doped oxidation lanthanum lutetium crystalline ceramics of holmium ytterbium and preparation method thereof |
| CN108329907A (en) * | 2018-03-27 | 2018-07-27 | 深圳科尔新材料科技有限公司 | Hard template sol-gal process prepares long-persistence luminous nano material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803974A (en) * | 2006-01-24 | 2006-07-19 | 中国科学院长春应用化学研究所 | Method for preparing oxide core shell structured spherical luminescent material |
-
2013
- 2013-01-04 CN CN2013100016147A patent/CN103074061A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803974A (en) * | 2006-01-24 | 2006-07-19 | 中国科学院长春应用化学研究所 | Method for preparing oxide core shell structured spherical luminescent material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105312558A (en) * | 2014-07-30 | 2016-02-10 | 苏州环球色谱有限责任公司 | Method for preparing core-shell type granules and application of core-shell type granules prepared with method |
| CN105312558B (en) * | 2014-07-30 | 2017-08-11 | 苏州环球色谱有限责任公司 | A kind of purposes of the method for preparing core-shell particle and its obtained core-shell particle |
| CN107619278A (en) * | 2017-10-25 | 2018-01-23 | 长春理工大学 | Double-doped oxidation lanthanum lutetium crystalline ceramics of holmium ytterbium and preparation method thereof |
| CN108329907A (en) * | 2018-03-27 | 2018-07-27 | 深圳科尔新材料科技有限公司 | Hard template sol-gal process prepares long-persistence luminous nano material |
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Application publication date: 20130501 |