CN100487075C - Method of preparing composite europium samarium stannate nano fluorescent powder - Google Patents
Method of preparing composite europium samarium stannate nano fluorescent powder Download PDFInfo
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- CN100487075C CN100487075C CNB2007100671862A CN200710067186A CN100487075C CN 100487075 C CN100487075 C CN 100487075C CN B2007100671862 A CNB2007100671862 A CN B2007100671862A CN 200710067186 A CN200710067186 A CN 200710067186A CN 100487075 C CN100487075 C CN 100487075C
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- europium
- stannate
- samarium
- nitrate
- fluorescent powder
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Abstract
The invention discloses a preparing method of europium samarium compound stannate nanometer luminescent powder, which comprises the following steps: dissolving diverse mole ratio azotic acid europium and azotic acid samarium in deionized water; adding into sodium stannate or postassium stannate; setting mole number as the sum of sodium stannate and postassium stannate; treating the allocating solution under 150-250 deg.c at 4-100 h with water and heat; setting filling degree at 80-90%; getting the product; setting the molecular formula as Eu2-xSmxSn2O7 and 0<x<2.0. The europium and samarium is normal rare earth luminescent activator, which can prepare compound stannate nanometer luminescent powder with controlling europium and samarium ratio at will and particle diameter at 20-60 nanometer.
Description
Technical field
The present invention relates to a kind of preparation method of composite europium samarium stannate nano fluorescent powder.
Background technology
Rare earth luminescent material has a extensive future in fields such as luminescent lamp, cathode ray tube (CRT), plasma flat-panel display (PDP) and X-ray detectors.Recent studies show that, nano-phosphor high resolution luminous with display device in have unique application.Therefore, the exploitation of novel rare-earth nano luminescent material has caused great interest.In various fluorescent materials, stannate is with 2000 ℃ of its stable chemical property, high fusing points (〉) and higher luminous efficiency high and quite paid close attention to.A lot of bibliographical informations the synthetic and luminescent properties of relevant stannate fluorescent material, as Ca
2SnO
4: Eu
3+(Y.C.Chen et al.Opt.Mater., 27,1874 (2005)), Sr
2SnO
4: Eu
3+(H.M.Yang et al.J.Alloy.Compd., 415,213 (2006)) and CaSnO
3: Eu
3+(Z.Lu et al.J.Alloy.Compd., 387, L1 (2005)) etc.Compare rare earth stannate (Ln with above-mentioned stannate
2Sn
2O
7(Ln=Y, La-Lu)) refers to a series of pyrochlore-type compounds, and they have application widely aspect lithium cell, catalyzer, ionophore and the radioprotective.Be easy to realize the doping of activator with rare earth stannate as the matrix of luminescent material, as Eu
3+, Sm
3+And Tb
3+Because atomic radius that it is close and similar electronic shell configuration, when mixing, can not cause the lattice distortion of matrix and not need charge compensation, they in addition can generate the compound rare-earth stannate.
The method of traditional preparation process pyrochlore-type rare earth stannate is very complicated, and these class methods are raw material with tindioxide and corresponding rare earth oxide mostly, carries out long solid state reaction under greater than 1400 ℃ high temperature to form.Than solid state reaction, hydrothermal synthesis method have equipment and simple to operate, reaction conditions is gentle, the product advantages of good crystallization, environmental pollution is little and characteristics such as suitable scale operation.In addition, hydrothermal method synthetic powder has high purity, high-crystallinity, grain-size is little, grain size distribution is narrow and advantage such as strict stoichiometric ratio.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of composite europium samarium stannate nano fluorescent powder.
The technical solution used in the present invention is that the step of this method is as follows:
1) different mol ratio europium nitrate and samaric nitrate are dissolved in the deionized water, the total mol concentration of control europium nitrate and samaric nitrate is 0.02～0.2 mol, stirs;
2) adding mole number again in above-mentioned solution is the sodium stannate or the potassium stannate of europium nitrate and samaric nitrate mole number sum, stirs;
3) solution that will finally prepare is put into autoclave, and compactedness is 80～90%, handles 4～100 hours in 150～250 ℃ of temperature ranges;
4) with solution centrifugal, the drying handled well, just obtained composite europium samarium stannate nano fluorescent powder Eu
2-xSm
xSn
2O
7, 0＜x＜2.0 wherein.
According to the preparation method of a kind of composite europium samarium stannate nano fluorescent powder of the present invention, be reactant with europium nitrate, samaric nitrate and sodium stannate or potassium stannate, by the synthetic composite europium samarium stannate nano fluorescent powder of hydrothermal method, molecular formula is Eu
2-xSm
xSn
2O
7, 0＜x＜2.0 wherein, particle is 20～60 nanometers, realizes that europium samarium ratio is controlled arbitrarily in the product, there is europium ion in product in 588～598 nanometer range
5D
0→
7F
1Luminous.
The beneficial effect that the present invention has is: be to be reactant with europium nitrate, samaric nitrate and sodium stannate or potassium stannate, (molecular formula is Eu to synthesize composite europium samarium stannate nano fluorescent powder by simple, neutral hydro-thermal technology
2-xSm
xSn
2O
7(0＜x＜2.0)), avoided the high temperature solid state reaction of traditional method; By controlling europium nitrate and the samaric nitrate ratio in the reactant easily, thereby controlled the ratio of europium samarium in the product effectively; The nano-phosphor particle diameter is 20～60 nanometers, and there is stronger europium ion in product in 588～598 nanometer range
5D
0→
7F
1Luminous.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1,2 and 3 gained composite europium samarium stannate nano fluorescent powders: (a) Eu
1.5Sm
0.5Sn
2O
7, (b) EuSmSn
2O
7, (c) Eu
0.5Sm
1.5Sn
2O
7
Fig. 2 is embodiment 1 products therefrom (Eu
1.5Sm
0.5Sn
2O
7) transmission electron microscope photo and electron diffraction pattern thereof;
Fig. 3 is embodiment 1 products therefrom (Eu
1.5Sm
0.5Sn
2O
7) the photoluminescence emmission spectrum;
Fig. 4 is embodiment 2 products therefrom (EuSmSn
2O
7) transmission electron microscope photo and electron diffraction pattern thereof;
Fig. 5 is embodiment 2 products therefrom (EuSmSn
2O
7) the photoluminescence emmission spectrum;
Fig. 6 is embodiment 3 products therefrom (Eu
0.5Sm
1.5Sn
2O
7) transmission electron microscope photo and electron diffraction pattern thereof;
Fig. 7 is embodiment 3 products therefrom (Eu
0.5Sm
1.5Sn
2O
7) the photoluminescence emmission spectrum.
Embodiment
Embodiment 1:
With 2.141 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 160 ml waters, europium nitrate volumetric molar concentration 0.03 mol stirred after 3 minutes, added 0.711 gram samaric nitrate (Sm (NO again
3)
36H
2O), samaric nitrate volumetric molar concentration 0.01 mol stirred after 3 minutes, added 1.914 gram potassium stannate (K again
2SnO
33H
2O), sodium stannate volumetric molar concentration 0.04 mol.Therefore, europium in the solution: samarium: the mol ratio of tin is 3:1:4, i.e. x=0.5.Stir after 5 minutes, the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, compactedness is 80%, and the liner volume is 200 milliliters.This solution was handled 24 hours down at 200 ℃, and solution centrifugal of handling well and drying, obtaining europium samarium ratio is the composite europium samarium stannate nano fluorescent powder (Eu of 3:1
1.5Sm
0.5Sn
2O
7).Fig. 1 (a) is the XRD figure spectrum of this nano rare earth fluorescent material, and the analysis revealed products therefrom is a typical cube of pyrochlore constitution, and its lattice parameter is
Fig. 2 is the transmission electron microscope photo of this routine products therefrom, and its particle diameter is about 20 nanometers.Fig. 3 is the photoluminescence emmission spectrum of product, Eu
3+Visible region exist corresponding to
5D
0→
7F
13 emission peaks of magnetic dipole transition are respectively 588,593,598 nanometers, send very strong safran fluorescence.Eu
3+609 and 617 nanometers exist corresponding to
5D
0-
7F
2The transition of electric dipole.Illustrate that this composite europium samarium stannate nano fluorescent powder has good luminescent properties.
Embodiment 2:
With 7.135 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 160 ml waters, europium nitrate volumetric molar concentration 0.10 mol stirred after 3 minutes, added 7.110 gram samaric nitrate (Sm (NO again
3)
36H
2O), europium nitrate volumetric molar concentration 0.10 mol stirred after 3 minutes, added 8.545 gram sodium stannate (Na again
2SnO
33H
2O), sodium stannate volumetric molar concentration 0.20 mol.Therefore, europium in the solution: samarium: the mol ratio of tin is 1:1:2, i.e. x=1.Stir after 5 minutes, the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, compactedness is 90%, and the liner volume is 200 milliliters.This solution was handled 100 hours down at 150 ℃, and solution centrifugal of handling well and drying, acquisition europium samarium ratio is 1: 1 composite europium samarium stannate nano fluorescent powder (EuSmSn
2O
7).Fig. 1 (b) is the XRD figure spectrum of this nano rare earth fluorescent material, and analysis revealed gained sample is typical case's cube pyrochlore constitution, and its lattice parameter is
Fig. 4 is the transmission electron microscope photo of this routine product, and its particle diameter is about 20 nanometers.Fig. 5 is the emmission spectrum of this example product, Eu
3+Visible region exist corresponding to
5D
0→
7F
13 emission peaks of magnetic dipole transition are respectively 588,593,598 nanometers, send safran fluorescence.Eu
3+609 and 617 nanometers exist corresponding to
5D
0-
7F
2The transition of electric dipole.Illustrate that this composite europium samarium stannate nano fluorescent powder has good luminescent properties.
Embodiment 3:
With 0.714 gram europium nitrate (Eu (NO
3)
36H
2O) be dissolved in 160 ml waters, lanthanum nitrate volumetric molar concentration 0.01 mol stirred after 3 minutes, added 2.133 gram samaric nitrate (Sm (NO again
3)
36H
2O), europium nitrate volumetric molar concentration 0.03 mol stirred after 3 minutes, added 1.709 gram sodium stannate (Na again
2SnO
33H
2O), sodium stannate volumetric molar concentration 0.04 mol.Therefore, europium in the solution: samarium: the mol ratio of tin is 1:1:2, i.e. x=1.5.Stir after 5 minutes, the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, compactedness is 80%, and the liner volume is 200 milliliters.This solution was handled 4 hours down at 250 ℃, and solution centrifugal of handling well and drying, obtaining europium samarium ratio is the composite europium samarium stannate nano fluorescent powder (Eu of 1:3
0.5Sm
1.5Sn
2O
7).Fig. 1 (c) is the XRD figure spectrum of this nano rare earth fluorescent material, and the analysis revealed products therefrom is typical case's letter cube pyrochlore constitution, and its lattice parameter is
Fig. 6 is the transmission electron microscope photo of this routine product, and particle diameter is about 60 nanometers.Fig. 7 is the emmission spectrum of this example product, Eu
3+Visible region exist corresponding to
5D
0→
7F
13 emission peaks of magnetic dipole transition are respectively 588,593,598 nanometers, send safran fluorescence.Eu
3+609 and 617 nanometers exist corresponding to
5D
0-
7F
2The transition of electric dipole.Illustrate that this composite europium samarium stannate nano fluorescent powder has good luminescent properties.
Claims (2)
1, a kind of preparation method of composite europium samarium stannate nano fluorescent powder is characterized in that the step of this method is as follows:
1) different mol ratio europium nitrate and samaric nitrate are dissolved in the deionized water, the total mol concentration of control europium nitrate and samaric nitrate is 0.02～0.2 mol, stirs;
2) adding mole number again in above-mentioned solution is the sodium stannate or the potassium stannate of europium nitrate and samaric nitrate mole number sum, stirs;
3) solution that will finally prepare is put into autoclave, and compactedness is 80～90%, handles 4～100 hours in 150～250 ℃ of temperature ranges;
4) with solution centrifugal, the drying handled well, just obtained composite europium samarium stannate nano fluorescent powder Eu
2-xSm
xSn
2O
7, 0＜x＜2.0 wherein.
2, the preparation method of a kind of composite europium samarium stannate nano fluorescent powder according to claim 1, it is characterized in that: with europium nitrate, samaric nitrate and sodium stannate or potassium stannate is reactant, by the synthetic composite europium samarium stannate nano fluorescent powder of hydrothermal method, molecular formula is Eu
2-xSm
xSn
2O
7, 0＜x＜2.0 wherein, particle is 20～60 nanometers, realizes that europium samarium ratio is controlled arbitrarily in the product, there is europium ion in product in 588～598 nanometer range
5D
0→
7F
1Luminous.
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| CN102051170B (en) * | 2009-11-02 | 2013-04-24 | 海洋王照明科技股份有限公司 | Calcium yttrium stannate light-emitting material doped with light-emitting ions and preparation method thereof |
| CN101824320A (en) * | 2010-05-19 | 2010-09-08 | 北京大学 | Red fluorescent powder, preparation method and application thereof |
| CN104556208B (en) * | 2015-01-19 | 2016-08-24 | 陕西科技大学 | A kind of spherical Sm2sn2o7nanocrystalline preparation method |
| CN104556211B (en) * | 2015-01-19 | 2016-06-29 | 陕西科技大学 | A kind of tin dope solvent thermal-hydro-thermal method prepares Sm2Sn2O7/SnO2The method of nano-complex |
| CN112745546A (en) * | 2020-12-28 | 2021-05-04 | 威海市泓淋电力技术股份有限公司 | Marine high-performance rubber and plastic sheath material and preparation process thereof |
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