CN103333689A - Method of thermosynthesis of SrWO4:Ln3<+> nanoribbon with solvent - Google Patents

Method of thermosynthesis of SrWO4:Ln3<+> nanoribbon with solvent Download PDF

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CN103333689A
CN103333689A CN2013102938962A CN201310293896A CN103333689A CN 103333689 A CN103333689 A CN 103333689A CN 2013102938962 A CN2013102938962 A CN 2013102938962A CN 201310293896 A CN201310293896 A CN 201310293896A CN 103333689 A CN103333689 A CN 103333689A
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solvent
srwo
nitrate
nano belt
synthesized
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王国凤
徐冰玉
李莹
潘清江
姚秀伟
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Heilongjiang University
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Heilongjiang University
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Abstract

The invention discloses a method of thermosynthesis of an SrWO4:Ln3<+> nanoribbon with a solvent, and relates to a synthetic method of the SrWO4:Ln3<+> nanoribbon. The method aims at obtaining the SrWO4:Ln3<+> nanoribbon. The method comprises the following steps of 1, adding a surfactant and anion salt to a strontium nitrate and rare-earth nitrate mixed solution, and stirring; 2, performing heat treatment; 3, washing and drying; and 4, roasting, and obtaining the SrWO4:Ln3<+> nanoribbon. The SrWO4:Ln3<+> nanoribbon is simple in preparation technology, low in cost, simple in required equipment, and high in production safety; industrial production is easy to realize; and the method is applied to the field of rare-earth optical functional materials.

Description

A kind of solvent thermal is synthesized SrWO 4: Ln 3+The method of nano belt
Technical field
The present invention relates to a kind of SrWO 4: Ln 3+The synthetic method of nano belt crystalline substance.
Background technology
Rare earth is the indispensable components of all multifunctional materials such as luminous, magnetics, superconduction, and the rare earth optical function material is widely used in fields such as terminal demonstration, opto-electronic device, laser technology and biology.Since people's reported first such as R.N.Bhargava in 1994 after the ZnS:Mn nano-crystalline granule has the quantum luminous efficiency that is higher than the body material, nano luminescent material has been subjected to the extensive concern of Chinese scholars.After the rare earth nanoization, show numerous characteristics, as small-size effect, high-ratio surface effect, quantum effect, extremely strong light, electricity, magnetic property, supraconductivity, high chemically reactive etc., can improve performance and the function of material greatly.Particularly the rare earth up-conversion luminescent material is widely used in biological and medical field.Compare with Quantum Dot Labeling with traditional organic dye, the rare earth up-conversion nano material has its special advantages.On the one hand, rare earth ion luminous has narrow emission band, high purity of color, long fluorescence lifetime and high characteristics such as anti-photobleaching.On the other hand, up-conversion nano material has no autofluorescence aspect biological fluorescent labelling disturbs, and biological tissue is not had injury, in advantages such as biological tissue's penetration depth are dark.
As everyone knows, the luminosity of rare earth ion is relevant with pattern and the size of nano material.Therefore, scholars are devoted to synthetic rare-earth nano-fluorescent material with special appearance.Up to the present, it is nanocrystalline that people have successfully synthesized series of rare earth by low-temperature hydrothermal, solvent thermal, microemulsion and original position method of substitution, comprises oxide compound, fluorochemical, vanadate and phosphoric acid salt etc.But, the present SrWO that does not also have special appearance 4: Ln 3+Nanocrystalline is synthetic.
Summary of the invention
Purpose of the present invention provides a kind of solvent thermal to synthesize SrWO 4: Ln 3+The method of nano belt.
A kind of solvent thermal of the present invention is synthesized SrWO 4: Ln 3+Nano belt is finished by following step: be that 40～90 ℃, stirring velocity are under 100～350r/min condition in temperature one,, in strontium nitrate and rare earth nitrate mixed solution, add tensio-active agent, add anion salt again, continuation is stirred 0.2～24h with the speed of 100～350r/min, gets mixture; Two, adopt solvent-thermal method that the mixture that step 1 obtains is heat-treated, get solution; Three, the solution that obtains with the distilled water wash step 2 is to pH=7, then vacuum-drying 3～24h under 60～80 ℃ of conditions; Four, in air, the desciccate of step 3 is carried out roasting, namely obtain SrWO 4: Ln 3+Nano belt; Wherein, the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:1～99, the selected solvent of solvent-thermal method is one or more mixing solutionss that mix by any ratio in water, dehydrated alcohol, the ethylene glycol in the step 2, the temperature that solvent-thermal method is handled is 110～220 ℃, and the solvent heat treatment time is 2～48h.
The described rare earth nitrate of step 1 is one or several mixtures by any ratio in europium nitrate, Erbium trinitrate, thulium nitrate, ytterbium nitrate, Dysprosium trinitrate, samaric nitrate, the Gadolinium trinitrate.
It is characterized in that tensio-active agent described in the step 1 comprises one or several mixtures by any ratio in cetyl trimethylammonium bromide, cetyl dimethyl benzyl ammonium bromide, sodium lauryl sulphate, sodium laurylsulfonate, hexadecyl dihydroxy ethyl amine oxide, octadecyl dimethyl amine oxide, octadecyl dihydroxy ethyl amine oxide, vinyl pyrrolidone, polyethylene glycol monooleate, hexadecanol, oleyl alcohol, the oleic acid.
Anion salt described in the step 1 is Na 2WO 4
Description of drawings
Fig. 1 is the SrWO of embodiment 22 preparations 4: Eu 3+Nanocrystalline transmission electron microscope photo;
Fig. 2 is the SrWO of embodiment 22 preparations 4: Eu 3+Nanocrystalline XRD spectrum;
Fig. 3 is the SrWO of embodiment 22 preparations 4: Eu 3+Nanocrystalline photoluminescence spectra.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of solvent thermal of present embodiment is synthesized SrWO 4: Ln 3+Nano belt is finished by following step:
One, be that 40～90 ℃, stirring velocity are under 100～350r/min condition in temperature, in strontium nitrate and rare earth nitrate mixed solution, add tensio-active agent, add anion salt again, continue to stir 0.2～24h with the speed of 100～350r/min, get mixture; Two, adopt solvent-thermal method that the mixture that step 1 obtains is heat-treated, get solution; Three, the solution that obtains with the distilled water wash step 2 is to pH=7, then vacuum-drying 3～24h under 60～80 ℃ of conditions; Four, in air, the desciccate of step 3 is carried out roasting, namely obtain SrWO 4: Ln 3+Nano belt; Wherein, the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:1～99, the selected solvent of solvent-thermal method is one or more mixing solutionss that mix by any ratio in water, dehydrated alcohol, the ethylene glycol in the step 2, the temperature that solvent-thermal method is handled is 110～220 ℃, and the solvent heat treatment time is 2～48h.
Embodiment two: what present embodiment and embodiment one were different is: the rare earth nitrate described in the step 1 is one or several mixtures by any ratio in europium nitrate, Erbium trinitrate, thulium nitrate, ytterbium nitrate, Dysprosium trinitrate, samaric nitrate, the Gadolinium trinitrate.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: tensio-active agent described in the step 1 is cetyl trimethylammonium bromide, cetyl dimethyl benzyl ammonium bromide, sodium lauryl sulphate, sodium laurylsulfonate, hexadecyl dihydroxy ethyl amine oxide, octadecyl dimethyl amine oxide, octadecyl dihydroxy ethyl amine oxide, vinyl pyrrolidone, polyethylene glycol monooleate, hexadecanol, oleyl alcohol, in the oleic acid one or more are by the mixture of any ratio.Other step and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different with one of embodiment one to three is: the anion salt described in the step 1 is Na 2WO 4Other step and parameter are identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one to four is: the temperature that solvent-thermal method adopts described in the step 2 is 150～200 ℃, and the solvent heat treatment time is 10～40h.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to five is: the temperature that solvent-thermal method adopts described in the step 2 is 160～190 ℃, and the solvent heat treatment time is 15～35h.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: the temperature that solvent-thermal method adopts described in the step 2 is 160～180 ℃, and the solvent heat treatment time is 20～30h.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different with one of embodiment one to seven is: the temperature that solvent-thermal method adopts described in the step 2 is 170 ℃, and the solvent heat treatment time is 25h.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different with one of embodiment one to eight is: the maturing temperature described in the step 4 is 200～900 ℃, and heat-up rate is 1～20 ℃/min, and roasting time is 0.05～8h.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different with one of embodiment one to nine is: the maturing temperature described in the step 4 is 300～800 ℃, and heat-up rate is 4～16 ℃/min, and roasting time is 0.5～7h.Other step and parameter are identical with one of embodiment one to nine.
Embodiment 11: what present embodiment was different with one of embodiment one to ten is: the maturing temperature described in the step 4 is 400～700 ℃, and heat-up rate is 6～15 ℃/min, and roasting time is 1～6h.Other step and parameter are identical with one of embodiment one to ten.
Embodiment 12: what present embodiment was different with one of embodiment one to 11 is: the maturing temperature described in the step 4 is 400～600 ℃, and heat-up rate is 8～15 ℃/min, and roasting time is 1～5h.Other step and parameter are identical with one of embodiment one to 11.
Embodiment 13: what present embodiment was different with one of embodiment one to 12 is: the maturing temperature described in the step 4 is 500 ℃, and heat-up rate is 10～12 ℃/min, and roasting time is 2～4h.Other step and parameter are identical with one of embodiment one to 12.
Embodiment 14: what present embodiment was different with one of embodiment one to 13 is: the concentration of the strontium nitrate described in the step 1 and rare earth nitrate mixed solution is 0.1～2mol/L.Other step and parameter are identical with one of embodiment one to 13.
Embodiment 15: what present embodiment was different with one of embodiment one to 14 is: the concentration of the strontium nitrate described in the step 1 and rare earth nitrate mixed solution is 0.5～1.5mol/L.Other step and parameter are identical with one of embodiment one to 14.
Embodiment 16: what present embodiment was different with one of embodiment one to 15 is: the concentration of the strontium nitrate described in the step 1 and rare earth nitrate mixed solution is 0.8～1.2mol/L.Other step and parameter are identical with one of embodiment one to 15.
Embodiment 17: what present embodiment was different with one of embodiment one to 16 is: the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:10～80.Other step and parameter are identical with one of embodiment one to 16.
Embodiment 18: what present embodiment was different with one of embodiment one to 17 is: the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:20～70.Other step and parameter are identical with one of embodiment one to 17.
Embodiment 19: what present embodiment was different with one of embodiment one to 18 is: the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:30～60.Other step and parameter are identical with one of embodiment one to 18.
Embodiment 20: what present embodiment was different with one of embodiment one to 19 is: the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:40～50.Other step and parameter are identical with one of embodiment one to 19.
Embodiment 21: what present embodiment was different with one of embodiment one to 20 is: the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:45.Other step and parameter are identical with one of embodiment one to 20.
Embodiment 22: a kind of solvent thermal of present embodiment is synthesized SrWO 4: Eu 3+Preparation of nano crystal is finished by following step: be that 40 ℃, stirring velocity are under the condition of 150r/min in temperature one,, add tensio-active agent PVP to the mixing solutions of strontium nitrate (99%) and europium nitrate (1%), add Na again 2WO 4Solution continues to stir 1 hour, and wherein said solvent is the mixing solutions of water and dehydrated alcohol; Two, with 140 ℃ of solvent heat treatment 24h of above-mentioned solution, get solution; Three, be washed with distilled water to the pH=7 of solution, vacuum-drying 10h under 80 ℃ of conditions obtains SrWO then 4: Eu 3+Nanocrystalline.The SrWO that present embodiment obtains 4: Eu 3+Nanocrystalline transmission electron microscope photo as shown in Figure 1, as can be seen from Figure 1 SrWO 4: Eu 3+Nanocrystalline particle size homogeneous.Fig. 2 is SrWO 4: Eu 3+Nanocrystalline XRD figure, as can be seen from the figure sample is the SrWO of pure cubic crystalline phase 4Fig. 3 is SrWO 4: Eu 3+Nanocrystalline photoluminescence spectra, as can be seen from the figure sample can send red fluorescence.

Claims (10)

1. a solvent thermal is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that solvent thermal synthesizes SrWO 4: Ln 3+The method of nano belt is carried out according to the following steps: be that 40～90 ℃, stirring velocity are under 100～350r/min condition in temperature one,, in strontium nitrate and rare earth nitrate mixed solution, add tensio-active agent, add anion salt again, continuation is stirred 0.2～24h with the speed of 100～350r/min, gets mixture; Two, adopt solvent-thermal method that the mixture that step 1 obtains is heat-treated, get solution; Three, the solution that obtains with the distilled water wash step 2 is to pH=7, then vacuum-drying 3～24h under 60～80 ℃ of conditions; Four, in air, the desciccate of step 3 is carried out roasting, namely obtain SrWO 4: Ln 3+Nano belt; Wherein, the mol ratio of the rare earth nitrate described in the step 1 and strontium nitrate is 1:1～99, the selected solvent of solvent-thermal method is one or more mixing solutionss that mix by any ratio in water, dehydrated alcohol, the ethylene glycol in the step 2, the temperature that solvent-thermal method is handled is 110～220 ℃, and the solvent heat treatment time is 2～48h.
2. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that the rare earth nitrate described in the step 1 is one or several mixtures by any ratio in europium nitrate, Erbium trinitrate, thulium nitrate, ytterbium nitrate, Dysprosium trinitrate, samaric nitrate, the Gadolinium trinitrate.
3. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that tensio-active agent described in the step 1 is one or more mixtures by any ratio in cetyl trimethylammonium bromide, cetyl dimethyl benzyl ammonium bromide, sodium lauryl sulphate, sodium laurylsulfonate, hexadecyl dihydroxy ethyl amine oxide, octadecyl dimethyl amine oxide, octadecyl dihydroxy ethyl amine oxide, vinyl pyrrolidone, polyethylene glycol monooleate, hexadecanol, oleyl alcohol, the oleic acid.
4. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that the anion salt described in the step 1 is Na 2WO 4
5. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that the temperature that solvent-thermal method adopts described in the step 2 is 150～200 ℃, and the solvent heat treatment time is 10～40h.
6. the method for the synthetic SrWO4:Ln3+ nano belt of a kind of solvent thermal according to claim 5 is characterized in that the temperature that solvent-thermal method adopts described in the step 2 is 160～180 ℃, and the solvent heat treatment time is 20～30h.
7. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that the maturing temperature described in the step 4 is 200～900 ℃, and heat-up rate is 1～20 ℃/min, and roasting time is 0.05～8h.
8. a kind of solvent thermal according to claim 7 is synthesized SrWO 4: Ln 3+The method of nano belt is characterized in that the maturing temperature described in the step 4 is 400～600 ℃, and heat-up rate is 8～15 ℃/min, and roasting time is 1～5h.
9. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt, the concentration that it is characterized in that the strontium nitrate described in the step 1 and rare earth nitrate mixed solution is 0.1～2mol/L.
10. a kind of solvent thermal according to claim 1 is synthesized SrWO 4: Ln 3+The method of nano belt, the mol ratio that it is characterized in that the rare earth nitrate described in the step 1 and strontium nitrate is 1:10～70.
CN2013102938962A 2013-07-11 2013-07-11 Method of thermosynthesis of SrWO4:Ln3<+> nanoribbon with solvent Pending CN103333689A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN106430311A (en) * 2016-09-12 2017-02-22 洛阳理工学院 Preparation method of strontium tungstate dendrite
CN106735166A (en) * 2016-12-12 2017-05-31 南京工业大学 A kind of EuWO4(OH) preparation method of nanobelt and its composite
CN116120929A (en) * 2022-09-30 2023-05-16 吉林建筑大学 Gd 3+ Fluorescent temperature measuring material for enhancing tungstate up-conversion luminescence and preparation method thereof

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN106430311A (en) * 2016-09-12 2017-02-22 洛阳理工学院 Preparation method of strontium tungstate dendrite
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CN116120929B (en) * 2022-09-30 2024-06-07 吉林建筑大学 Gd3+Fluorescent temperature measuring material for enhancing tungstate up-conversion luminescence and preparation method thereof

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Application publication date: 20131002