CN102061172A - Europium (Eu) ion doped Y7O6F9 nanobelt and preparation method thereof - Google Patents
Europium (Eu) ion doped Y7O6F9 nanobelt and preparation method thereof Download PDFInfo
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- CN102061172A CN102061172A CN 201010550215 CN201010550215A CN102061172A CN 102061172 A CN102061172 A CN 102061172A CN 201010550215 CN201010550215 CN 201010550215 CN 201010550215 A CN201010550215 A CN 201010550215A CN 102061172 A CN102061172 A CN 102061172A
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Abstract
The invention relates to a europium (Eu) ion doped Y7O6F9 nanobelt and a preparation method thereof, belonging to the technical field of nano material preparation. Rare-earth fluoride nanobelts are prepared by the existing electrospinning technology. The method comprises the following three steps: (1) preparing a Y2O3:5%Eu3+nanobelt: preparing a composite PVP/[Y(NO3)3+Eu(NO3)3] nanobelt by adopting the electrospinning technology and then carrying out heat treatment on the composite nanobelt to obtain the Y2O3:5%Eu3+nanobelt; (2) preparing a YF3:5%Eu3+nanobelt: taking ammonium bifluoride as a fluorinating reagent and fluorinating the Y2O3:5%Eu3+nanobelt by a double crucible method to obtain the YF3:5%Eu3+nanobelt; and (3) preparing a Y7O6F9:5%Eu3+nanobelt: placing the YF3:5%Eu3+nanobelt into a muffle furnace and heating the YF3:5%Eu3+nanobelt in air atmosphere at the temperature of 580 DEG C for 9 hours to obtain the Y7O6F9:5%Eu3+nanobelt. The Y7O6F9:5%Eu3+nanobelt has the width of 1.9-3.7 mu m, thickness of 185nm and length of more than 300 mu m. The Eu ion doped Y7O6F9 nanobelt is a novel important red nano fluorescent material and has a broad application prospect.
Description
Technical field
The present invention relates to the nano material preparation technical field, relate to europium ion-doped Y specifically
7O
6F
9Nano belt and preparation method thereof.
Background technology
The preparation of inorganics nano belt and property research are one of forward position focus of subject researchs such as Materials science, Condensed Matter Physics, chemistry at present.Nano belt is a kind ofly to be the nano material of zonal structure with the manual method synthetic, and its cross section is a rectangular configuration, and its thickness is in nanometer scale, and width can reach micron order, and length can reach the hundreds of micron, even several millimeters.Nano belt is different from performances such as the novel structure of pipe, wire material and unique light, electricity, magnetic and causes people's great attention owing to it.
The rare earth oxyfluoride phonon energy is low, and higher luminous quantum efficiency is arranged, and has good thermostability and environmental stability, extensively is used as luminescent material matrix.Europium ion-doped fluorine yttrium oxide (Y
7O
6F
9: Eu
3+) be important red fluorescence material.At present, do not see that Y is arranged
7O
6F
9: Eu
3+The relevant report of nano material.Y
7O
6F
9: Eu
3+Nano belt is a kind of important novel red nano luminescent material, will obtain important application in fields such as luminous and demonstration, false proof, biomarker, nano-devices, has broad application prospects.Do not see Y at present
7O
6F
9: Eu
3+The report of nano belt.
The patent No. technical scheme of a relevant electrospinning process (electrospinning) that has been 1975504 U.S. Patent Publication, this method is the preparation successive, has a kind of effective ways of the micro nanometer fiber of macro length, at first proposed in 1934 by Formhals.This method is mainly used to prepare high polymer nanometer fiber, it is characterized in that making charged macromolecular solution or melt in electrostatic field, to be subjected to the traction of electrostatic force and spray by nozzle, invest the receiving screen on opposite, thereby realization wire drawing, then, solvent evaporation at normal temperatures, perhaps melt is cooled to normal temperature and solidifies, and obtains micro nanometer fiber.Over nearly 10 years, occurred adopting electrospinning process to prepare the technical scheme of mineral compound such as oxidate nano fiber at the inorganic fibre preparing technical field, described oxide compound comprises TiO
2, ZrO
2, Y
2O
3, Y
2O
3: RE
3+(RE
3+=Eu
3+, Tb
3+, Er
3+, Yb
3+/ Er
3+), NiO, Co
3O
4, Mn
2O
3, Mn
3O
4, CuO, SiO
2, Al
2O
3, V
2O
5, ZnO, Nb
2O
5, MoO
3, CeO
2, LaMO
3(M=Fe, Cr, Mn, Co, Ni, Al), Y
3Al
5O
12, La
2Zr
2O
7Deng metal oxide and composite oxide of metal.Existing people utilizes electrostatic spinning technique successfully to prepare high molecular nanometer band (Materials Letters, 2007,61:2325-2328; Journal of PolymerScience:Part B:Polymer Physics, 2001,39:2598-2606).Someone utilizes the organic compound of tin, uses electrostatic spinning technique to combine with the organometallics decomposition technique and has prepared porous SnO
2Nano belt (Nanotechnology, 2007,18:435704); Someone utilizes electrostatic spinning technique at first to prepare PEO/ stannic hydroxide composite Nano band, and its roasting has been obtained porous SnO
2Nano belt (J.Am.Ceram.Soc., 2008,91 (1): 257-262).Employing electrostatic spinning techniques such as Dong Xiangting prepared rare earth fluoride nanobelt (Chinese invention patent, application number: 201010108039.7), titanium dioxide nano-belts (Chinese invention patent, ZL200810050948.2) and Gd
3Ga
5O
12: Eu
3+Porous nano-belt (SCI, 2010,31 (7), 1291-1296).At present, do not see Y
7O
6F
9: Eu
3+The report of nano belt.
When utilizing electrostatic spinning technique to prepare nano material, the composition of the kind of raw material, the molecular weight of high polymer templates, spinning solution, spinning process parameter and thermal treatment process all have material impact to the pattern and the size of the finished product.The present invention adopts electrostatic spinning technique earlier, with yttrium oxide (Y
2O
3) and europium sesquioxide (Eu
2O
3) be raw material, with evaporating behind the dilute nitric acid dissolution, obtain Y (NO
3)
3And Eu (NO
3)
3Mixed crystal adds solvent N, and dinethylformamide (DMF) and high polymer templates polyvinylpyrrolidone (the PVP molecular weight is 1300000) obtain carrying out electrostatic spinning behind the spinning solution, under the experiment condition of the best, prepare PVP/[Y (NO
3)
3+ Eu (NO
3)
3] original nano belt, it is heat-treated in air, obtain Y
2O
3: Eu
3+Nano belt adopts double crucible method to fluoridize the YF that has obtained pure phase
3: Eu
3+Nano belt; In air, heat-treat again, prepared the Y of novel structure
7O
6F
9: Eu
3+Nano belt.
Summary of the invention
Use electrostatic spinning technique in background technology has prepared metal oxide, composite oxide of metal nanofiber, high molecular nanometer band, SnO
2Nano belt, TiO
2Nano belt, Gd
3Ga
5O
12: Eu
3+Porous nano-belt and rare earth fluoride nanobelt.In order to provide a kind of in the nano belt field is the novel red Illuminant nanometer band of matrix with the rare earth oxyfluoride, and we have invented Y
7O
6F
9: Eu
3+Nano belt and preparation method thereof.
The present invention is achieved in that and at first prepares the spinning solution with certain viscosity that is used for electrostatic spinning, uses electrostatic spinning technique and carries out electrostatic spinning, under the experiment condition of the best, prepares PVP/[Y (NO
3)
3+ Eu (NO
3)
3] original nano belt, it is heat-treated in air, obtain Y
2O
3: Eu
3+Nano belt adopts double crucible method to fluoridize the YF that has prepared pure phase
3: Eu
3+Nano belt; In air, heat-treat again, prepare the Y of the pure phase of novel structure
7O
6F
9: Eu
3+Nano belt, in the present invention, the molecular fraction of adulterated europium ion is 5%, is labeled as Y
7O
6F
9: 5%Eu
3+, i.e. that the present invention is prepared is Y
7O
6F
9: 5%Eu
3+Nano belt.The steps include:
(1) preparation Y
2O
3: 5%Eu
3+Nano belt
That use in yttrium source and europium source is yttrium oxide (Y
2O
3) and europium sesquioxide (Eu
2O
3), high polymer templates adopts polyvinylpyrrolidone (PVP, molecular weight are 1300000), adopts N, and dinethylformamide (DMF) is a solvent.Take by weighing a certain amount of yttrium oxide and europium sesquioxide, both mol ratios are 19: 1, and promptly the molecular fraction of europium ion is 5%, with evaporating behind the dilute nitric acid dissolution, obtain Y (NO
3)
3And Eu (NO
3)
3Mixed crystal adds in an amount of DMF solvent, takes by weighing a certain amount of PVP again and joins in the above-mentioned solution, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, promptly forms spinning solution.The mass percent of this each integral part of spinning solution is: rare earth nitrate content 18%, PVP content 18%, solvent DMF content 64%.The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, nozzle diameter 0.7mm, the angle of adjusting nozzle and horizontal plane is 15 °, applies the volts DS of 13kV, solidifies apart from 15cm, 18～25 ℃ of room temperatures, relative humidity is 50%～70%, obtains PVP/[Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band.With described PVP/[Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band is put in the temperature programmed control stove and heat-treats, temperature rise rate is 1 ℃/min, at 700 ℃ of constant temperature 8h, naturally cools to room temperature with body of heater afterwards, promptly obtains Y
2O
3: 5%Eu
3+Nano belt.
(2) preparation YF
3: 5%Eu
3+Nano belt
Fluorination reagent uses ammonium bifluoride, adopts double crucible method, with described Y
2O
3: 5%Eu
3+Nano belt is put into crucible, adds excessive ammonium bifluoride between interior outer crucible, adds that on outer crucible the crucible lid carries out fluoridation, at 280 ℃ of insulation 2h, is warmed up to 450 ℃ of thermal treatment 3h again, and temperature rise rate is 2 ℃/min, obtains YF3:5%Eu
3+Nano belt.
(3) preparation Y
7O
6F
9: 5%Eu
3+Nano belt
With YF
3: 5%Eu
3+Nano belt is placed in the muffle furnace, in 580 ℃ of heating 9h, obtains Y in air atmosphere
7O
6F
9: 5%Eu
3+Nano belt, bandwidth are 1.9～3.7 μ m, and thickness is 185nm, and length is greater than 300 μ m.
At the Y described in the said process
7O
6F
9: 5%Eu
3+The bandwidth of nano belt is 1.9～3.7 μ m, and thickness is 185nm, and length has realized goal of the invention greater than 300 μ m.
Description of drawings
Fig. 1 is Y
7O
6F
9: 5%Eu
3+The XRD spectra of nano belt;
Fig. 2 is Y
7O
6F
9: 5%Eu
3+The SEM photo of nano belt, this figure double as Figure of abstract;
Fig. 3 is Y
7O
6F
9: 5%Eu
3+The EDS spectrogram of nano belt;
Fig. 4 is Y
7O
6F
9: 5%Eu
3+The exciting light spectrogram of nano belt;
Fig. 5 is Y
7O
6F
9: 5%Eu
3+The emmission spectrum figure of nano belt.
Embodiment
Yttrium oxide (the Y that the present invention is selected
2O
3) and europium sesquioxide (Eu
2O
3) purity be 99.99%, polyvinylpyrrolidone (PVP, molecular weight 1300000), N, dinethylformamide (DMF), ammonium bifluoride (NH
4HF
2) and nitric acid (HNO
3) be commercially available analytical pure product; Used glassware and equipment are instrument and equipments commonly used in the laboratory.
Embodiment: take by weighing 1g Y
2O
3With 0.0820g Eu
2O
3, both mol ratios are 19: 1, promptly the molecular fraction of europium ion is 5%, with evaporating behind the dilute nitric acid dissolution, obtains Y (NO
3)
3And Eu (NO
3)
3Mixed crystal adds 9.2178g DMF solvent, adds 2.5925g PVP again in above-mentioned solution, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, promptly forms spinning solution.The mass percent of this each integral part of spinning solution is: rare earth nitrate content 18%, PVP content 18%, solvent DMF content 64%.The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, nozzle diameter 0.7mm, the angle of adjusting nozzle and horizontal plane is 15 °, applies the volts DS of 13kV, solidifies apart from 15cm, 18～25 ℃ of room temperatures, relative humidity is 50%～70%, obtains PVP/[Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band.With described PVP/[Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band is put in the temperature programmed control stove and heat-treats, temperature rise rate is 1 ℃/min, at 700 ℃ of constant temperature 8h, naturally cools to room temperature with body of heater afterwards, promptly obtains Y
2O
3: 5%Eu
3+Nano belt.Fluorination reagent uses ammonium bifluoride, adopts double crucible method, with described Y
2O
3: 5%Eu
3+Nano belt is put into crucible, adds excessive ammonium bifluoride between interior outer crucible, adds that on outer crucible the crucible lid carries out fluoridation, at 280 ℃ of insulation 2h, is warmed up to 450 ℃ of thermal treatment 3h again, and temperature rise rate is 2 ℃/min, obtains YF
3: 5%Eu
3+Nano belt.With YF
3: 5%Eu
3+Nano belt is placed in the muffle furnace, in 580 ℃ of heating 9h, obtains Y in air atmosphere
7O
6F
9: 5%Eu
3+Nano belt.Described Y
7O
6F
9: 5%Eu
3+Nano belt has good crystallinity, the d value of its diffraction peak and relative intensity and Y
7O
6F
9The listed d value of PDF standard card (80-1126) consistent with relative intensity, belong to rhombic system, see shown in Figure 1.Described Y
7O
6F
9: 5%Eu
3+The bandwidth of nano belt is 1.9～3.7 μ m, and thickness is 185nm, and length is seen shown in Figure 2 greater than 300 μ m.Y
7O
6F
9: 5%Eu
3+Nano belt is seen shown in Figure 3 by Y, O, F and Eu elementary composition (the Au conductive layer of surface plating when Au comes from the SEM sample preparation).When the monitoring wavelength is 615nm, Y
7O
6F
9: 5%Eu
3+The excitation spectrum highest peak of nano belt is positioned at the 254nm place, belongs to O
2--Eu
3+Between the charge migration band, see shown in Figure 4.Under the ultraviolet excitation of 254nm, Y
7O
6F
9: 5%Eu
3+Nano belt is launched the bright red that main peak is positioned at 615nm, and it is corresponding to Eu
3+Ionic
5D
0→
7F
2Transition belongs to Eu
3+Force electric dipole transition, see shown in Figure 5.
Certainly; the present invention also can have other various embodiments; under the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art work as can make various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (6)
1. europium ion-doped Y
7O
6F
9Nano belt and preparation method thereof is characterized in that, adopts electrostatic spinning technique, use polyvinylpyrrolidone (PVP) to be high polymer templates, adopt N, dinethylformamide (DMF) is a solvent, fluorination reagent uses ammonium bifluoride, and the preparation product is europium ion-doped Y
7O
6F
9Nano belt the steps include:
(1) preparation Y
2O
3: 5%Eu
3+Nano belt
That use in yttrium source and europium source is yttrium oxide (Y
2O
3) and europium sesquioxide (Eu
2O
3), high polymer templates adopts polyvinylpyrrolidone, adopts N, dinethylformamide is a solvent, takes by weighing a certain amount of yttrium oxide and europium sesquioxide, and both mol ratios are 19: 1, the molecular fraction that is europium ion is 5%, with evaporating behind the dilute nitric acid dissolution, obtains Y (NO
3)
3And Eu (NO
3)
3Mixed crystal, add in an amount of DMF solvent, taking by weighing a certain amount of PVP again joins in the above-mentioned solution, stir 4h in the room temperature lower magnetic force, and leave standstill 2h, promptly form spinning solution, the mass percent of this each integral part of spinning solution is: rare earth nitrate content 18%, PVP content 18%, solvent DMF content 64% adds the spinning solution for preparing in the liquid storage pipe of device for spinning, carry out electrostatic spinning, nozzle diameter 0.7mm, the angle of adjusting nozzle and horizontal plane is 15 °, applies the volts DS of 13kV, curing is apart from 15cm, 18～25 ℃ of room temperatures, relative humidity is 50%～70%, obtains PVP/[Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band, with described PVP/[Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band is put in the temperature programmed control stove and heat-treats, temperature rise rate is 1 ℃/min, at 700 ℃ of constant temperature 8h, naturally cools to room temperature with body of heater afterwards, promptly obtains Y
2O
3: 5%Eu
3+Nano belt;
(2) preparation YF
3: 5%Eu
3+Nano belt
Fluorination reagent uses ammonium bifluoride, adopts double crucible method, with described Y
2O
3: 5%Eu
3+Nano belt is put into crucible, adds excessive ammonium bifluoride between interior outer crucible, adds that on outer crucible the crucible lid carries out fluoridation, at 280 ℃ of insulation 2h, is warmed up to 450 ℃ of thermal treatment 3h again, and temperature rise rate is 2 ℃/min, obtains YF
3: 5%Eu
3+Nano belt;
(3) preparation Y
7O
6F
9: 5%Eu
3+Nano belt
With YF
3: 5%Eu
3+Nano belt is placed in the muffle furnace, in 580 ℃ of heating 9h, obtains Y in air atmosphere
7O
6F
9: 5%Eu
3+Nano belt, bandwidth are 1.9～3.7 μ m, and thickness is 185nm, and length is greater than 300 μ m.
2. europium ion-doped Y according to claim 1
7O
6F
9Nano belt and preparation method thereof is characterized in that, that use in yttrium source and europium source is yttrium oxide (Y
2O
3) and europium sesquioxide (Eu
2O
3).
3. europium ion-doped Y according to claim 1
7O
6F
9Nano belt and preparation method thereof is characterized in that, high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=1300000.
4. europium ion-doped Y according to claim 1
7O
6F
9Nano belt and preparation method thereof is characterized in that, solvent adopts N, dinethylformamide.
5. europium ion-doped Y according to claim 1
7O
6F
9Nano belt and preparation method thereof is characterized in that, fluorination reagent uses ammonium bifluoride.
6. europium ion-doped Y according to claim 1
7O
6F
9Nano belt and preparation method thereof is characterized in that, adulterated Eu
3+Molecular fraction is 5%.
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605470A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Preparation method of europium-doped Y4Al2O9 red light-emitting nanobelt |
| CN102605469A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Method for preparing Eu (europium)-doped Y4Al2O9 red luminescent nano fiber |
| CN102618969A (en) * | 2012-02-24 | 2012-08-01 | 长春理工大学 | Preparation method of europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt |
| CN102660806A (en) * | 2012-02-24 | 2012-09-12 | 长春理工大学 | Method for preparing europium-doped LiYF4 nanofiber |
| CN102660803A (en) * | 2012-02-24 | 2012-09-12 | 长春理工大学 | Method for preparing europium-doped yttrium lithium tetrafluoride (YLF) nanobelt |
| CN102817113A (en) * | 2012-08-10 | 2012-12-12 | 长春理工大学 | Preparation method of terbium-doped octafluoro yttrium barium green luminescent nano-fiber |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102605470A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Preparation method of europium-doped Y4Al2O9 red light-emitting nanobelt |
| CN102605469A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Method for preparing Eu (europium)-doped Y4Al2O9 red luminescent nano fiber |
| CN102618969A (en) * | 2012-02-24 | 2012-08-01 | 长春理工大学 | Preparation method of europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt |
| CN102660806A (en) * | 2012-02-24 | 2012-09-12 | 长春理工大学 | Method for preparing europium-doped LiYF4 nanofiber |
| CN102660803A (en) * | 2012-02-24 | 2012-09-12 | 长春理工大学 | Method for preparing europium-doped yttrium lithium tetrafluoride (YLF) nanobelt |
| CN102660803B (en) * | 2012-02-24 | 2014-01-15 | 长春理工大学 | Method for preparing europium-doped yttrium lithium tetrafluoride (YLF) nanobelt |
| CN102618969B (en) * | 2012-02-24 | 2014-02-12 | 长春理工大学 | Preparation method of europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt |
| CN102660806B (en) * | 2012-02-24 | 2014-06-25 | 长春理工大学 | Method for preparing europium-doped LiYF4 nanofiber |
| CN102817113A (en) * | 2012-08-10 | 2012-12-12 | 长春理工大学 | Preparation method of terbium-doped octafluoro yttrium barium green luminescent nano-fiber |
| CN102817113B (en) * | 2012-08-10 | 2014-07-02 | 长春理工大学 | Preparation method of terbium-doped octafluoro yttrium barium green luminescent nano-fiber |
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