CN101157473A - Preparation method of rare-earth doping fluoride nano luminescent particles - Google Patents
Preparation method of rare-earth doping fluoride nano luminescent particles Download PDFInfo
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- CN101157473A CN101157473A CNA2007100462195A CN200710046219A CN101157473A CN 101157473 A CN101157473 A CN 101157473A CN A2007100462195 A CNA2007100462195 A CN A2007100462195A CN 200710046219 A CN200710046219 A CN 200710046219A CN 101157473 A CN101157473 A CN 101157473A
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Abstract
The invention relates to a method for preparing nanometer luminescent particles of rare earth doping fluoride, LnF3:RE<3+>. The method comprises the following procedures: firstly, preparing rare-earth element RE containing polyalcohol solutions of Ln nitride and NH4F as raw reaction liquid; secondly, loading the reaction liquid into a syringe and propelling with a micro-amount propulsion pump into a micro mixer for mixing, and then entering the mixture into a microcapillary and heating with a constant-temperature oil bath to synthesize polyalcohol dispersion liquid of LnF3:RE<3+> nanometer luminescent particles; thirdly, performing further extraction, washing and centrifugal separation to obtain the LnF3:RE<3+> nanometer luminescent particles. The method has simple synthesis technology and facilitates batch production. The prepared LnF3: RE<3+> nanometer luminescent particles have small size, excellent dispersibility, narrow diameter distribution and favorable luminance.
Description
Technical field
The invention belongs to rare earth mixing with nano luminophore field, particularly relate to a kind of rare-earth-doped fluoride (LnF
3: RE
3+) preparation method of nano luminescent particles.
Background technology
Rare earth dopen Nano luminophore is a kind of important fluorescent material, its kind is abundant, spectral qualities is high, synthetic method is versatile and flexible, application at aspects such as laser apparatus, fiber amplifier and three dimensional display and anti-counterfeiting technologies has obtained gratifying achievement, is expected to be applied in organism fluorescent mark aspect simultaneously.Because LaF
3Have low phonon energy, high thermostability and environmental stability, and all rare earth ions are all had very strong solvability make LaF
3Become good solid electrolyte, electrode materials, good optical substrate material.CeF
3Faraday effect, in photoelectronics, had applicability, for example optoisolator, optical switch and optical memory.CeF
3Nano particle presents high Faraday effect and have low absorption under visible light and makes it become the material that qualified magnetooptics is used.Compare with traditional oxidation matrix luminescent material, fluorochemical has low vibrational energy, and the quencher of energy minimization rare earth ion excited state.Therefore, fluorochemical has the superiority as rare earth doping body material.
What the preparation method of rare-earth-doped fluoride used always has: the precipitator method, sol-gel method, chemical gas phase synthetic method, hydrothermal method etc.Germany S.Eiden-Assmann at Materials Research Bulletin, 2004,39, reported on the 21-24 that employing polyolefin method has prepared CeF
3Nano particle.The H.GUO of department of physics of Zhejiang Normal University is at Appl.Phys.B, and 2006,84, the CeF that reported employing hydro-thermal prepared with microemulsion reactor on the 365-369
3: Tb
3+The nanometer video disc; The D.Y.Kong of Changchun applied chemistry institute is at Nanotechnology, and 2007,18, reported with the glycol ether to be that solvent has prepared CeF on the 1-7
3: Tb
3+Nano particle.The Z.L.Wang of Changchun applied chemistry institute has reported on the 2030-2037 that at Chem.Mater.2006 employing polyolefin method has prepared CeF
3: Tb
3+/ LaF
3The nano particle of nucleocapsid structure.But the nano particle of above preparation but its preparation process complexity, and nonaqueous phase are used for biomarker and need carry out finishing.In a word, traditional preparation method need high-temperature calcination or in oil phase high temperature synthetic, in the aqueous solution, easily reunite.Directly the synthetic crystallization nano particle has important significance for theories and practical value in water or alcoholic solvent.
Microreactor is the chemical reaction system that a kind of unit process interface width is the microminiaturization of micron dimension, is little chemical industry technology of rising the nineties.It often uses with little heat transfer technology, little hybrid technology.The microreactor that is reduced to of physical size brings advantage, and it mainly acts on is to the reinforcement of quality and heat transfer process and the aspects such as improvement of fluid-flow mode.Therefore, what microreactor was mainly strengthened is transfer characteristic, and in liquid phase reaction, reaction liquid is a laminar flow regime, and diffusion is the main path of mass transfer.Japan Hiroyuki Nakamura is at Lab Chip, and 2004,4, reported on the 237-240 that diameter is that the silex glass microcapillary temperature of 200 μ m only is 0.28s from 20 ℃ of times that are heated to 300 ℃ of needs, has promptly fully proved the heat-transfer capability of microreactor.Microreactor has following characteristics: 1. flowing in the passage is laminar flow; 2. specific surface area is big, and heat-transfer capability is strong, and temperature control is easy; 3. molecular diffusion is apart from weak point, and mass transfer is fast; 4. can realize " number increases amplification ", no scale effect.Contrivers etc. are at Adv.Funct.Mater.2005, and 15 (4): reported preparation CdSe-ZnS composite nanometer particle in the employing microreactor on 603-608. and the Chem.commun.2004:48-49..Up to the present, the research of relevant microreactor middle-weight rare earths doping fluoride nano luminescent particles does not appear in the newspapers.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of rare-earth doping fluoride nano luminescent particles, this method adopts microreactor, has synthesized rear-earth-doped LnF in polyhydric alcohol solutions
3Nano luminescent particles is grown up by changing reaction times control particulate, can make have narrow size distribution, the light-emitting particles of excellent dispersion properties, strong fluorescence property.
Rare-earth-doped fluoride (LnF of the present invention
3: RE
3+) preparation method of nano luminescent particles, comprise the following steps:
(1) the nitric acid Ln polyhydric alcohol solutions and the NH of preparation doped with rare-earth elements RE solution
4The F polyhydric alcohol solutions is as reaction stoste;
(2) reaction solution is packed into syringe adopts micro-boost pump to push micro mixer and mixes, and enters microcapillary, by the constant temperature oil bath reacting by heating, and synthetic rare earth doped fluorochemical (LnF
3: RE
3+) the polyvalent alcohol dispersion liquid of nano luminescent particles;
(3) further extraction, washing, centrifugation get rare-earth-doped fluoride (LnF
3: RE
3+) nano luminescent particles.
Described polyvalent alcohol is ethylene glycol, glycerine or Diethylene Glycol;
Described nitric acid Ln polyhydric alcohol solutions is 0.001～0.1mol/L La (NO
3)
36H
2O or Ce (NO
3)
36H
2The polyhydric alcohol solutions of O;
Described doped with rare-earth elements RE solution is 0.001～0.1mol/L Eu
2O
3, Ce (NO
3)
36H
2O, Tb (NO
3)
36H
2In the O polyhydric alcohol solutions a kind of, two or three, adulterated mol ratio is La
3+: RE
3+=3.5: 6.5～9.5: 0.5 or Ce
3+: RE
3+=3.5: 6.5～9.5: 0.5;
Described NH
4The concentration of F polyhydric alcohol solutions is 0.001-0.1mol/L;
The diameter of described microcapillary is 200-1000 μ m, and length is 0.01-3m, and material comprises tetrafluoroethylene, glass etc.;
Described constant temperature oil bath reacting by heating is that temperature is 50-190 ℃, reaction 1s-30min;
Described extraction is by organic solvents such as adding acetone or alcohols, produces precipitation;
Described washing is to adopt organic solvent washing such as acetone or alcohol 3-5 time;
Described centrifugation is the centrifugal 2-40min of 2000-8000rpm.
Beneficial effect of the present invention:
(1) can synthesize and contain the adulterated fluoride nano luminescent particles of different rare earth ions;
(2) synthetic rare-earth-doped fluoride (LnF
3: RE
3+) size of nano luminescent particles is little, good dispersity, narrow size distribution, good luminous performance;
(3) simple, the required production unit of synthesis technique is simple, is easy to produce in batches.
Description of drawings
Fig. 1 is LaF
3: Ce
3+, Tb
3+The X-ray diffractogram of nano luminescent particles;
Fig. 2 is LaF
3: Ce
3+, Tb
3+The transmission electron microscope photo of nano luminescent particles;
Fig. 3 is LaF
3: Ce
3+, Tb
3+The excitation-emission spectrum of nano luminescent particles;
Fig. 4 is CeF
3: Tb
3+The X-ray diffractogram of nano luminescent particles;
Fig. 5 is CeF
3: Tb
3+The transmission electron microscope photo of nano luminescent particles;
Fig. 6 is CeF
3: Tb
3+The high-resolution-ration transmission electric-lens photo of nano luminescent particles;
Fig. 7 is CeF
3: Tb
3+The excitation-emission spectrum of nano luminescent particles.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing 0.2600g La (NO
3)
36H
2O joins in the 100mL ethylene glycol solution, and magnetic agitation is until dissolving; Take by weighing 0.1302gCe (NO
3)
36H
2O, 0.0454gTb (NO
3)
36H
2O adds above-mentioned solution, and magnetic agitation obtains containing Ln until dissolving
3+(Ln=La, Ce, Tb) the glycol reaction stoste of 0.01mol/L, wherein La
3+: Ce
3+: Tb
3+=6: 3: 1 (mol ratio).Take by weighing 0.111gNH
4F joins in the 100mL ethylene glycol solution, and magnetic agitation obtains the NH of 0.01mol/L until dissolving
4F glycol reaction stoste.Then two reaction stostes are joined in the two isodiametric syringes, prevent leakage with the estersil sealing, with micro-boost pump reaction solution is pushed in the micro mixer to mix and laggardly go into microcapillary (diameter is 200 μ m, length is 0.15m, material is a glass) in, reaction is 20 minutes in 80 ℃ constant temperature oil bath, and reaction finishes the back and receives product with sample bottle, obtains Ce
3+, Tb
3+Doping LaF
3The ethylene glycol dispersion liquid of nano luminescent particles.Add acetone in the product that obtains until producing precipitation, then in whizzer under the 4500rpm rotating speed from getting 20 minutes.Again be scattered in the acetone from the precipitation of getting and precipitate so that same rotating speed is centrifugal again, wash that drying obtains LaF under the product room temperature after three times
3: Ce
3+, Tb
3+Nano luminescent particles.Fig. 1 is present embodiment synthetic LaF
3: Ce
3+, Tb
3+The X-ray diffractogram of nano luminescent particles can be seen belonging to six side's phase LaF
3Diffraction peak, illustrate and synthesized LaF
3: Ce
3+, Tb
3+Nano luminescent particles.Fig. 2 is its transmission electron microscope photo, shows its synthetic LaF
3: Ce
3+, Tb
3+Nano luminescent particles is a class spheric particle, and granular size is in the 10nm, narrow size distribution, and even particle distribution.Fig. 3 is synthetic LaF
3: Ce
3+, Tb
3+The excitation-emission spectrum of nano luminescent particles ethylene glycol dispersion liquid, LaF as can be seen
3: Ce
3+, Tb
3+Nano luminescent particles has certain fluorescent properties.
Embodiment 2
Take by weighing 0.3474g Ce (NO
3)
36H
2O joins in the 100mL ethylene glycol solution, and magnetic agitation is until dissolving; Take by weighing 0.0906gTb (NO
3)
36H
2O joins in the above-mentioned solution, and magnetic agitation obtains containing Ln until dissolving
3+(Ln=Ce, Tb) the glycol reaction stoste of 0.01mol/L, wherein Ce
3+: Tb
3+=4: 1 (mol ratio).Take by weighing 0.111gNH
4F joins in the 100mL ethylene glycol solution, and magnetic agitation obtains the NH of 0.01moL/L until dissolving
4F glycol reaction stoste.Then two reaction stostes are joined in the two isodiametric syringes, prevent leakage with the estersil sealing, with micro-boost pump reaction solution is pushed in the micro mixer to mix and laggardly go into microcapillary (diameter is 200 μ m, length is 0.15m, material is a tetrafluoroethylene) in, reaction is 30 minutes in 50 ℃ constant temperature oil bath, and reaction finishes the back and receives product with sample bottle, obtains Tb
3+Doped Ce F
3The ethylene glycol dispersion liquid of nano luminescent particles.Add acetone in the product that obtains until producing precipitation, then in whizzer under the 2000rpm rotating speed from getting 40 minutes.Again be scattered in the acetone from the precipitation of getting and precipitate so that same rotating speed is centrifugal again, dry CeF under the product room temperature after acetone is given a baby a bath on the third day after its birth time
3: Tb
3+Nano luminescent particles.Fig. 4 is present embodiment synthetic CeF
3: Tb
3+The X-ray diffractogram of nano luminescent particles can be seen belonging to six side's phase CeF
3Diffraction peak, illustrate and synthesized CeF
3: Tb
3+Nano luminescent particles.Fig. 5 is its transmission electron microscope photo, shows its synthetic CeF
3: Tb
3+Nano luminescent particles is a class spheric particle, and granular size is in the 10nm, narrow size distribution, and even particle distribution.Fig. 6 is its high-resolution-ration transmission electric-lens photo, has showed its synthetic CeF
3: Tb
3+The character striped of nano luminescent particles shows CeF
3: Tb
3+Nano luminescent particles has high crystallinity.Fig. 7 is synthetic CeF
3: Tb
3+The excitation-emission spectrum of nano luminescent particles ethylene glycol dispersion liquid, CeF as can be seen
3: Tb
3+Nano luminescent particles has certain fluorescent properties.
Take by weighing 0.3246g La (NO
3)
36H
2O joins in the 100mL ethylene glycol solution, and magnetic agitation is until dissolving; Take by weighing 0.1086gCe (NO
3)
36H
2O joins in the above-mentioned solution, and magnetic agitation obtains containing Ln until dissolving
3+(Ln=La, Ce) the glycol reaction stoste of 0.01mol/L, wherein La
3+: Ce
3+=3: 1 (mol ratio).Take by weighing 0.111gNH
4F joins in the 100mL ethylene glycol solution, and magnetic agitation obtains the NH of 0.01moL/L until dissolving
4F glycol reaction stoste.Then two reaction stostes are joined in the two isodiametric syringes, prevent leakage with the estersil sealing, with micro-boost pump reaction solution is pushed in the micro mixer to mix and laggardly go into microcapillary (diameter is 500 μ m, length is 0.1m, material is a glass) in, reaction is 5 minutes in 190 ℃ constant temperature oil bath, and reaction finishes the back and receives product with sample bottle, obtains Ce
3+Doping LaF
3The ethylene glycol dispersion liquid of nano luminescent particles.Add ethanol in the product that obtains until producing precipitation, then in whizzer under the 8000rpm rotating speed from getting 2 minutes.Again be scattered in the ethanol from the precipitation of getting and precipitate so that same rotating speed is centrifugal again, dry LaF under the product room temperature after ethanol is given a baby a bath on the third day after its birth time
3: Ce
3+Nano luminescent particles.The X ray test result of spreading out shows that synthetic is LaF
3: Ce
3+Nano luminescent particles.Transmission electron microscope observing shows that its particle size is little, is uniformly dispersed.
Take by weighing 0.2600g La (NO
3)
36H
2O joins in the 100mL ethylene glycol solution, and magnetic agitation is until dissolving; Take by weighing 0.1812gTb (NO
3)
36H
2O joins in the above-mentioned solution, and magnetic agitation obtains containing Ln until dissolving
3+(Ln=La, Tb) the glycol reaction stoste of 0.01mol/L, wherein La
3+: Tb
3+=3: 2 (mol ratios).Take by weighing 0.111gNH
4F joins in the 100mL ethylene glycol solution, and magnetic agitation obtains the NH of 0.01moL/L until dissolving
4F glycol reaction stoste.Then two reaction stostes are joined in the two isodiametric syringes, prevent leakage with the estersil sealing, with micro-boost pump reaction solution is pushed in the micro mixer to mix and laggardly go into microcapillary (diameter is 1000 μ m, length is 0.05m, material is a glass) in, reaction is 15 minutes in 100 ℃ constant temperature oil bath, and reaction finishes the back and receives product with sample bottle, obtains Tb
3+Doping LaF
3The ethylene glycol solution of nano luminescent particles.Add acetone in the product that obtains until producing precipitation, then in whizzer under the 6000rpm rotating speed from getting 10 minutes.Again be scattered in the acetone from the precipitation of getting and precipitate so that same rotating speed is centrifugal again, dry LaF under the product room temperature after acetone is given a baby a bath on the third day after its birth time
3: Ce
3+Nano luminescent particles.The X ray test result of spreading out shows that synthetic is LaF
3: Tb
3+Nano luminescent particles.Transmission electron microscope observing shows that its particle size is little, is uniformly dispersed.
Embodiment 5
Take by weighing 0.3474g Ce (NO
3)
36H
2O joins in the 100mL glycerine solution, and magnetic agitation is until dissolving; Take by weighing 0.0906gTb (NO
3)
36H
2O joins in the above-mentioned solution, and magnetic agitation obtains containing Ln until dissolving
3+(Ln=Ce, Tb) the glycerine reaction stoste of 0.01mol/L, wherein Ce
3+: Tb
3+=4: 1 (mol ratio).Take by weighing 0.111gNH
4F joins in the 100mL glycerine solution, and magnetic agitation obtains the NH of 0.01moL/L until dissolving
4F glycerine reaction stoste.Then two reaction stostes are joined in the two isodiametric syringes, prevent leakage with the estersil sealing, with micro-boost pump reaction solution is pushed in the micro mixer to mix and laggardly go into microcapillary (diameter is 1000 μ m, length is 0.05m, material is a tetrafluoroethylene) in, reaction is 10 minutes in 120 ℃ constant temperature oil bath, and reaction finishes the back and receives product with sample bottle, obtains Tb
3+Doped Ce F
3The glycerine dispersion liquid of nano luminescent particles.Add acetone in the product that obtains until producing precipitation, then in whizzer under the 3000rpm rotating speed from getting 30 minutes.Again be scattered in the acetone from the precipitation of getting and precipitate so that same rotating speed is centrifugal again, dry CeF under the product room temperature after acetone is given a baby a bath on the third day after its birth time
3: Tb
3+Nano luminescent particles.The X ray test result of spreading out shows that synthetic is CeF
3: Tb
3+Nano luminescent particles.Transmission electron microscope observing shows that its particle size is little, is uniformly dispersed.
Embodiment 6
Take by weighing 0.3908g Ce (NO
3)
36H
2O joins in the 100mL Diethylene Glycol solution, and magnetic agitation is until dissolving; Take by weighing 0.0176gEu
2O
3, the dense HNO of 0.0278g
3Join in the above-mentioned solution, magnetic agitation obtains containing RE until dissolving
3+(RE=Eu, La) reaction of the Diethylene Glycol of 0.01mol/L stoste, wherein Eu
3+: Ce
3+=1: 9 (mol ratios); Take by weighing 0.111gNH
4F joins in the 100mL Diethylene Glycol solution, and magnetic agitation obtains the NH of 0.01mol/L until dissolving
4F Diethylene Glycol reaction stoste.Two kinds of reaction solutions are joined respectively in two isodiametric syringes, prevent leakage with the estersil sealing.With micro-boost pump reaction solution is pushed in the micro mixer, solution mixes laggardly goes into microcapillary (diameter is 800 μ m, and length is 0.1m, material is a tetrafluoroethylene) in, reaction is 25 minutes in 80 ℃ constant temperature oil bath, and reaction finishes the back and receives product with sample bottle, obtains CeF
3: Eu
3+The Diethylene Glycol dispersion liquid of nano luminescent particles.Add acetone in the product that obtains until producing precipitation, then in whizzer under the 4500rpm rotating speed from getting 15 minutes.Again be scattered in the acetone from the precipitation of getting and must precipitate so that same rotating speed is centrifugal again, under the product room temperature after acetone is given a baby a bath on the third day after its birth time in dry CeF
3: Eu
3+Nano luminescent particles.The X ray test result of spreading out shows that synthetic is CeF
3: Eu
3+Nano luminescent particles.Transmission electron microscope observing shows that its particle size is little, is uniformly dispersed.
Claims (10)
1. rare-earth-doped fluoride LnF
3: RE
3+The preparation method of nano luminescent particles comprises the following steps:
(1) the nitric acid Ln polyhydric alcohol solutions and the NH of preparation doped with rare-earth elements RE solution
4The F polyhydric alcohol solutions is as reaction stoste;
(2) reaction solution is packed into syringe adopts micro-boost pump to push micro mixer and mixes, and enters microcapillary, by the constant temperature oil bath reacting by heating, and synthetic rare earth doped fluorochemical LnF
3: RE
3+The polyvalent alcohol dispersion liquid of nano luminescent particles;
(3) further extraction, washing, centrifugation get rare-earth-doped fluoride LnF
3: RE
3+Nano luminescent particles.
2. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described polyvalent alcohol is ethylene glycol, glycerine or Diethylene Glycol.
3. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described nitric acid Ln polyhydric alcohol solutions is 0.001～0.1mol/L La (NO
3)
36H
2O or Ce (NO
3)
36H
2The polyhydric alcohol solutions of O.
4. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described doped with rare-earth elements RE solution is 0.001～0.1mol/L Eu
2O
3, Ce (NO
3)
36H
2O, Tb (NO
3)
36H
2In the O polyhydric alcohol solutions a kind of, two or three, adulterated mol ratio is La
3+: RE
3+=3.5: 6.5～9.5: 0.5 or Ce
3+: RE
3+=3.5: 6.5～9.5: 0.5.
5. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described NH
4The concentration of F polyhydric alcohol solutions is 0.001-0.1mol/L.
6. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: the diameter of described microcapillary is 200-1000 μ m, and length is 0.01-3m, and material is tetrafluoroethylene or glass.
7. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described constant temperature oil bath reacting by heating is that temperature is 50-190 ℃, reacts 1 second-30 minutes.
8. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described extraction is by adding the acetone or alcohol organic solvent, producing precipitation.
9. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described washing is to adopt the acetone or alcohol organic solvent washing 3-5 time.
10. rare-earth-doped fluoride LnF according to claim 1
3: RE
3+The preparation method of nano luminescent particles is characterized in that: described centrifugation is the centrifugal 2-40min of 2000-8000rpm.
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|---|---|---|---|
| CNA2007100462195A CN101157473A (en) | 2007-09-20 | 2007-09-20 | Preparation method of rare-earth doping fluoride nano luminescent particles |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942932A (en) * | 2012-11-15 | 2013-02-27 | 中国科学院西安光学精密机械研究所 | Preparation method of rare earth doped fluoride nano dispersion liquid |
| CN103074064A (en) * | 2013-01-30 | 2013-05-01 | 东华大学 | Preparation method of rare-earth doped phosphate LnPO4:RE<3+> luminous nanoparticle |
| CN106350068A (en) * | 2016-08-30 | 2017-01-25 | 四川省有色冶金研究院有限公司 | Cerium-europium-terbium codoped nanocrystal fluorescent powder and preparation method thereof |
| CN106753379A (en) * | 2016-11-10 | 2017-05-31 | 哈尔滨理工大学 | A kind of preparation method of terbium ion doping fluoride solid luminescent material |
| CN110699728A (en) * | 2019-09-10 | 2020-01-17 | 桂林理工大学 | Rare earth trifluoride LnF3Film and preparation method thereof |
| CN112456536A (en) * | 2020-11-12 | 2021-03-09 | 西南大学 | Solid electrolyte material, fluorine ion battery and preparation method thereof |
-
2007
- 2007-09-20 CN CNA2007100462195A patent/CN101157473A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942932A (en) * | 2012-11-15 | 2013-02-27 | 中国科学院西安光学精密机械研究所 | Preparation method of rare earth doped fluoride nano dispersion liquid |
| CN102942932B (en) * | 2012-11-15 | 2014-01-29 | 中国科学院西安光学精密机械研究所 | Preparation method of rare earth doped fluoride nano dispersion liquid |
| CN103074064A (en) * | 2013-01-30 | 2013-05-01 | 东华大学 | Preparation method of rare-earth doped phosphate LnPO4:RE<3+> luminous nanoparticle |
| CN106350068A (en) * | 2016-08-30 | 2017-01-25 | 四川省有色冶金研究院有限公司 | Cerium-europium-terbium codoped nanocrystal fluorescent powder and preparation method thereof |
| CN106350068B (en) * | 2016-08-30 | 2018-07-06 | 四川省有色冶金研究院有限公司 | A kind of cerium europium terbium co-doped nano crystalline substance fluorescent powder and preparation method thereof |
| CN106753379A (en) * | 2016-11-10 | 2017-05-31 | 哈尔滨理工大学 | A kind of preparation method of terbium ion doping fluoride solid luminescent material |
| CN110699728A (en) * | 2019-09-10 | 2020-01-17 | 桂林理工大学 | Rare earth trifluoride LnF3Film and preparation method thereof |
| CN110699728B (en) * | 2019-09-10 | 2022-02-18 | 桂林理工大学 | Rare earth trifluoride LnF3Film and preparation method thereof |
| CN112456536A (en) * | 2020-11-12 | 2021-03-09 | 西南大学 | Solid electrolyte material, fluorine ion battery and preparation method thereof |
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