CN102817113B - Preparation method of terbium-doped octafluoro yttrium barium green luminescent nano-fiber - Google Patents
Preparation method of terbium-doped octafluoro yttrium barium green luminescent nano-fiber Download PDFInfo
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- CN102817113B CN102817113B CN201210283286.XA CN201210283286A CN102817113B CN 102817113 B CN102817113 B CN 102817113B CN 201210283286 A CN201210283286 A CN 201210283286A CN 102817113 B CN102817113 B CN 102817113B
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Abstract
The invention relates to a preparation method of terbium-doped octafluoro yttrium barium green luminescent nano-fiber, and belongs to the technical field of nano-grade material preparation. The method comprises four steps that: (1) a spinning liquid is prepared; (2) PVP/[Ba(NO3)2+Y(NO3)3+Tb(NO3)3] composite fiber is prepared with an electro-spinning technology; (3) mixed oxide nano-fiber is prepared, wherein the composite fiber is subjected to a heat treatment, such that the mixed oxide nano-fiber is prepared; and (4) BaY2F8:5% Tb<3+> green luminescent nano-fiber is prepared, wherein a double-crucible method is adopted, and the mixed oxide nano-fiber is subjected to a fluorination treatment by using ammonium bifluoride, such that the BaY2F8:5% Tb<3+> green luminescent nano-fiber is prepared. The nano-fiber has good crystallinity, a diameter of 113.9nm (plus or minus 8.7nm), and a length greater than 50mum. The method provided by the invention is simple and feasible, and can be used in batch productions. Therefore, the method has good application prospect.
Description
Technical field
The present invention relates to nano material preparation research field, relate to specifically the preparation method who mixes terbium octafluoro yttrium baryta green look luminous nano fibre.
Background technology
Nanofiber refers to the filamentary material of bidimensional in nanoscale on the three dimensions yardstick of material, and radial dimension is nanometer scale conventionally, and length is larger.Because the radial dimension of nanofiber is little of nanometer scale, demonstrate series of characteristics, the most outstanding is that specific area is large, thereby its surface can increase with active, and then produce small-size effect, surface or interfacial effect, quantum size effect, macro quanta tunnel effect etc., and therefore show the specificity of a series of chemistry, physics (heat, light, sound, electricity, magnetic etc.) aspect.In the prior art, there is the method for much preparing nanofiber, the method for for example reeling off raw silk from cocoons, template synthetic method, split-phase method and self-assembly method etc.In addition, also has arc evaporation, laser high temperature inustion, compound pyrolysismethod.These three kinds of methods are in fact all at high temperature to make after compound (or simple substance) evaporation, make nanofiber or nanotube through pyrolysis (or directly condensation), from essence, all belong to compound steam sedimentation.
Rare earth octafluoro compound, owing to having abundant 4f energy level and lower phonon energy, is one of current efficient rare-earth ion doping luminous host.Mix terbium octafluoro yttrium barium BaY
2f
8: Tb
3+be a kind of important green luminescent material, there is important application prospect.At present, BaY
2f
8: Tb
3+powder body material mainly adopts the methods such as high temperature solid-state method, hydro-thermal and solvent-thermal method, sol-gel process, microemulsion method, microwave method, combustion method, laser ablation method, presoma pyrolysismethod to synthesize, and synthetic product is BaY
2f
8: Tb
3+micron particles or nano particle.Mix terbium octafluoro yttrium barium BaY
2f
8: Tb
3+nanofiber is a kind of novel green luminescent material, will obtain important application in fields such as luminous and demonstration, false proof, medical science detection, biomarker, solar cell, chemistry and biology sensor, nano-devices, has broad application prospects.At present, have no and mix terbium octafluoro yttrium barium BaY
2f
8: Tb
3+the report of nanofiber.
The patent No. is that 1975504 United States Patent (USP) discloses a technical scheme about electrospinning process (electrospinning), the method is to prepare a kind of effective ways of continuous, to have macro length micro nanometer fiber, is first proposed in 1934 by Formhals.This method is mainly used to prepare high polymer nanometer fiber, it is characterized in that making charged Polymer Solution or melt in electrostatic field, are subject to the traction of electrostatic force and are sprayed by nozzle, invest the receiving screen on opposite, thereby realize wire drawing, then, solvent evaporation at normal temperatures, or melt cooling solidifies to normal temperature, obtains micro nanometer fiber.Over nearly 10 years, occurred adopting electrospinning process to prepare inorganic compound as the technical scheme of oxidate nano fiber at inorfil preparing technical field, described oxide 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.The employing electrostatic spinning techniques such as Wang Jinxian have been prepared rare earth fluoride/rare earth oxyfluoride composite nano fibre (Chinese invention patent, grant number: ZL200810050959.0); The employing electrostatic spinning techniques such as Dong Xiangting have been prepared and have been mixed europium Y
7o
6f
9nanofiber (Chinese invention patent, grant number: ZL201010550196.3); The employing electrostatic spinning techniques such as Wang Jinxian have been prepared trifluorides nanofiber (Chinese invention patent, grant number: ZL201010107993.4); Wang Ce etc. adopt electrostatic spinning technique to pass through R (CF
3cO
2)
3/ PVP (R=Eu, Ho) composite nano fiber is heat-treated, and has synthesized ROF (R=Eu, Ho) nanofiber (J.Nanosci.Nanotechnol., 2009,9 (2): 1522-1525).Electrospinning process can continuous production big L/D ratio micrometer fibers or nanofiber.Have no at present to adopt electrostatic spinning technique to combine with fluorination technology to prepare and mix terbium octafluoro yttrium barium BaY
2f
8: Tb
3+the report of green emitting nanofiber.
While 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 Technology for Heating Processing pattern and the size to final products has material impact.The present invention first adopts electrostatic spinning technique, with yittrium oxide Y
2o
3with terbium oxide Tb
4o
7for raw material, with evaporating after nitric acid dissolve, obtain yttrium nitrate Y (NO
3)
3with terbium nitrate Tb (NO
3)
3mixed crystal, adds barium nitrate Ba (NO
3)
2, solvent DMF DMF and high polymer templates polyvinylpyrrolidone PVP, obtain carrying out electrostatic spinning after spinning solution, under best experiment condition, prepare PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre, it is heat-treated in air, obtain mixed oxide nanoparticle fiber, adopt double crucible method, with ammonium acid fluoride NH
4hF
2fluoridize for fluorization agent, prepared the BaY of novel structure pure phase
2f
8: Tb
3+green emitting nanofiber.
Summary of the invention
In the various methods of preparing nanofiber in background technology, the shortcoming of the method for reeling off raw silk from cocoons is that solution viscosity is required to too harshness; The shortcoming of template synthetic method is to prepare the continuous fibers that root root separates; Split-phase method and self-assembly method production efficiency are all lower; And compound steam sedimentation is due to the demand to high temperature, so process conditions are difficult to control, and nanofiber major diameter prepared by above-mentioned several method is than little.Use electrostatic spinning technique in background technology has been prepared metal oxide, composite oxide of metal nanofiber, rare earth fluoride/rare earth oxyfluoride composite nano fibre, has been mixed europium Y
7o
6f
9nanofiber, trifluorides nanofiber and ROF (R=Eu, Ho) nanofiber.Prior art adopts the methods such as high temperature solid-state method, hydro-thermal and solvent-thermal method, sol-gel process, microemulsion method, microwave method, combustion method, laser ablation method, presoma pyrolysismethod to synthesize BaY
2f
8: Tb
3+micron particles or nano particle.For a kind of novel green luminous nano fibre material is provided in nanofiber field, we combine electrostatic spinning technique with fluorination technology, invented BaY
2f
8: Tb
3+the preparation method of green emitting nanofiber.
The present invention is achieved in that the spinning solution with certain viscosity of first preparing for electrostatic spinning, and application electrostatic spinning technique carries out electrostatic spinning, under best experiment condition, prepares PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre, it is heat-treated in air, obtained mixed oxide nanoparticle fiber, adopt double crucible method, with ammonium acid fluoride NH
4hF
2fluoridize for fluorization agent, prepared the BaY of novel structure pure phase
2f
8: Tb
3+green emitting nanofiber.In the present invention, the mole percent of the terbium ion of doping is 5%, is labeled as BaY
2f
8: 5%Tb
3+, i.e. that the present invention is prepared is BaY
2f
8: 5%Tb
3+green emitting nanofiber.The steps include:
(1) preparation spinning solution
That barium source is used is barium nitrate Ba (NO
3)
2, that He Te source, yttrium source is used is yittrium oxide Y
2o
3with terbium oxide Tb
4o
7, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 90000, and adopting DMF DMF is solvent, takes a certain amount of barium nitrate Ba (NO
3)
2, yittrium oxide Y
2o
3with terbium oxide Tb
4o
7, wherein Ba
2+, Y
3+and Tb
3+mol ratio be 50: 95: 5, the mole percent of terbium ion is 5%, by yittrium oxide Y
2o
3with terbium oxide Tb
4o
7use nitric acid HNO
3after dissolving, evaporation, obtains Y (NO
3)
3and Tb (NO
3)
3mixed crystal, adds barium nitrate Ba (NO
3)
2, DMF DMF solvent and polyvinylpyrrolidone PVP, stir 4h in room temperature lower magnetic force, and standing 2h, forming spinning solution, the mass percent of the each part of this spinning solution is: nitrate content 9%, PVP content 12%, solvent DMF content 79%;
(2) prepare PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre
The spinning solution preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, the angle of adjusting shower nozzle and horizontal plane is 15 °, apply the DC voltage of 15kY, solidify apart from 16cm 20～28 DEG C of room temperatures, relative humidity is 45%～75%, obtains PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre;
(3) prepare mixed oxide nanoparticle fiber
By described PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre is put in temperature programmed control stove and heat-treats, heating rate is 1 DEG C/min, at 700 DEG C of constant temperature 8h, then is cooled to 200 DEG C with the speed of 1 DEG C/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle fiber;
(4) prepare BaY
2f
8: 5%Tb
3+green emitting nanofiber
Fluorination reagent uses ammonium acid fluoride NH
4hF
2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle fiber is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add appropriate ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, be warming up to 280 DEG C of insulation 2h with the heating rate of 2 DEG C/min, then be warmed up to 700 DEG C of insulation 4h, be finally cooled to 200 DEG C with the rate of temperature fall of 1 DEG C/min, naturally cool to room temperature with body of heater afterwards, obtain BaY
2f
8: 5%Tb
3+green emitting nanofiber, diameter is 113.9 ± 8.7nm, length is greater than 50 μ m.
At the BaY described in said process
2f
8: 5%Tb
3+green emitting nanofiber has good crystallinity, and diameter is 113.9 ± 8.7nm, and length is greater than 50 μ m, has realized goal of the invention.
Brief description of the drawings
Fig. 1 is BaY
2f
8: 5%Tb
3+the XRD spectra of green emitting nanofiber;
Fig. 2 is BaY
2f
8: 5%Tb
3+the SEM photo of green emitting nanofiber, this figure doubles as Figure of abstract;
Fig. 3 is BaY
2f
8: 5%Tb
3+the diameter distribution histogram of green emitting nanofiber;
Fig. 4 is BaY
2f
8: 5%Tb
3+the exciting light spectrogram of green emitting nanofiber;
Fig. 5 is BaY
2f
8: 5%Tb
3+the utilizing emitted light spectrogram of green emitting nanofiber.
Detailed description of the invention
The yittrium oxide Y that the present invention is selected
2o
3with terbium oxide Tb
4o
7purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 90000, DMF DMF, carbon-point, barium nitrate Ba (NO
3)
2, ammonium acid fluoride NH
4hF
2with nitric acid HNO
3be commercially available analysis net product; Glass apparatus, crucible and equipment used is instrument and equipment conventional in laboratory.
Embodiment: take a certain amount of barium nitrate Ba (NO
3)
2, yittrium oxide Y
2o
3with terbium oxide Tb
4o
7, wherein Ba
2+, Y
3+and Tb
3+mol ratio be 50: 95: 5, the mole percent of terbium ion is 5%, by yittrium oxide Y
2o
3with terbium oxide Tb
4o
7use nitric acid HNO
3after dissolving, evaporation, obtains Y (NO
3)
3and Tb (NO
3)
3mixed crystal, adds barium nitrate Ba (NO
3)
2, DMF DMF solvent and polyvinylpyrrolidone PVP, stir 4h in room temperature lower magnetic force, and standing 2h, forming spinning solution, the mass percent of the each part of this spinning solution is: nitrate content 9%, PVP content 12%, solvent DMF content 79%; The spinning solution preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, the angle of adjusting shower nozzle and horizontal plane is 15 °, apply the DC voltage of 15kV, solidify apart from 16cm 20～28 DEG C of room temperatures, relative humidity is 45%～75%, obtains PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre; By described PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre is put in temperature programmed control stove and heat-treats, heating rate is 1 DEG C/min, at 700 DEG C of constant temperature 8h, then is cooled to 200 DEG C with the speed of 1 DEG C/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle fiber; Fluorination reagent uses ammonium acid fluoride NH
4hF
2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle fiber is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add appropriate ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, be warming up to 280 DEG C of insulation 2h with the heating rate of 2 DEG C/min, then be warmed up to 700 DEG C of insulation 4h, be finally cooled to 200 DEG C with the rate of temperature fall of 1 DEG C/min, naturally cool to room temperature with body of heater afterwards, obtain BaY
2f
8: 5%Tb
3+green emitting nanofiber.Described BaY
2f
8: 5%Tb
3+green emitting nanofiber, has good crystallinity, the d value of its diffraction maximum and relative intensity and BaY
2f
8the listed d value of PDF standard card (45-0246) consistent with relative intensity, belong to monoclinic system, as shown in Figure 1.Described BaY
2f
8: 5%Tb
3+the diameter of green emitting nanofiber is even, is fibrous, and length is greater than 50 μ m, as shown in Figure 2.By Shapiro-Wilk method to BaY
2f
8: 5%Tb
3+the diameter of green emitting nanofiber carries out normal distribution-test, under 95% confidence level, and BaY
2f
8: 5%Tb
3+the diameter of green emitting nanofiber distributes and belongs to normal distribution, and diameter is 113.9 ± 8.7nm, as shown in Figure 3.In the time that monitoring wavelength is 543nm, BaY
2f
8: 5%Tb
3+the strongest excitation peak of nanofiber is positioned at 369nm place, corresponding to Tb
3+'s
7f
6→
5d
3transition, as shown in Figure 4.Under the ultraviolet excitation of 369nm, BaY
2f
8: 5%Tb
3+nanofiber is launched main peak and is positioned at the bright green glow of 543nm, corresponding to Tb
3+ion
5d
4→
7f
5transition, as shown in Figure 5.
Certainly; the present invention also can have other various embodiments; in the situation that not deviating from spirit of the present invention and essence thereof; those of ordinary skill in the art are when making according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (1)
1. mix the preparation method of terbium octafluoro yttrium baryta green look luminous nano fibre, it is characterized in that, the method that adopts electrostatic spinning technique to combine with fluorination technology, using the polyvinylpyrrolidone PVP of molecular weight Mr=90000 is high polymer templates, adopt N, dinethylformamide DMF is solvent, and fluorination reagent uses ammonium acid fluoride NH
4hF
2, preparing product is terbium ion doping octafluoro yttrium barium BaY
2f
8: 5%Tb
3+green emitting nanofiber, the steps include:
(1) preparation spinning solution
That barium source is used is barium nitrate Ba (NO
3)
2, that He Te source, yttrium source is used is yittrium oxide Y
2o
3with terbium oxide Tb
4o
7, high polymer templates adopts polyvinylpyrrolidone PVP, and adopting DMF DMF is solvent, takes a certain amount of barium nitrate Ba (NO
3)
2, yittrium oxide Y
2o
3with terbium oxide Tb
4o
7, wherein Ba
2+, Y
3+and Tb
3+mol ratio be 50:95:5, the mole percent of terbium ion is 5%, by yittrium oxide Y
2o
3with terbium oxide Tb
4o
7use nitric acid HNO
3after dissolving, evaporation, obtains Y (NO
3)
3and Tb (NO
3)
3mixed crystal, adds barium nitrate Ba (NO
3)
2, DMF DMF solvent and polyvinylpyrrolidone PVP, stir 4h in room temperature lower magnetic force, and standing 2h, forming spinning solution, the mass percent of the each part of this spinning solution is: nitrate content 9%, PVP content 12%, solvent DMF content 79%;
(2) prepare PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre
The spinning solution preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, the angle of adjusting shower nozzle and horizontal plane is 15 °, apply the DC voltage of 15kV, solidify apart from 16cm 20～28 DEG C of room temperatures, relative humidity is 45%～75%, obtains PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre;
(3) prepare mixed oxide nanoparticle fiber
By described PVP/[Ba (NO
3)
2+ Y (NO
3)
3+ Tb (NO
3)
3] composite fibre is put in temperature programmed control stove and heat-treats, heating rate is 1 DEG C/min, at 700 DEG C of constant temperature 8h, then is cooled to 200 DEG C with the speed of 1 DEG C/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle fiber;
(4) prepare BaY
2f
8: 5%Tb
3+green emitting nanofiber
Fluorination reagent uses ammonium acid fluoride NH
4hF
2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle fiber is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add appropriate ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, be warming up to 280 DEG C of insulation 2h with the heating rate of 2 DEG C/min, then be warmed up to 700 DEG C of insulation 4h, be finally cooled to 200 DEG C with the rate of temperature fall of 1 DEG C/min, naturally cool to room temperature with body of heater afterwards, obtain BaY
2f
8: 5%Tb
3+green emitting nanofiber, diameter is 113.9 ± 8.7nm, length is greater than 50 μ m.
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|---|---|---|---|
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|---|---|---|---|
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| CN104059668A (en) * | 2013-03-21 | 2014-09-24 | 海洋王照明科技股份有限公司 | Terbium/ytterbium double-doped alkaline earth sodium yttrium fluoride up-conversion luminescent material, preparation method and organic light-emitting diode |
| CN104562183B (en) * | 2014-12-31 | 2018-01-19 | 西南技术物理研究所 | Large scale rare-earth adulterates yttrium fluoride barium method for monocrystal growth |
| CN106120023B (en) * | 2016-07-04 | 2018-05-22 | 长春理工大学 | A kind of method for preparing er-doped yttrium fluoride barium up-conversion luminescence nanofiber |
| CN113957566B (en) * | 2021-11-20 | 2023-07-07 | 福州大学 | Solid oxide battery composite nanofiber and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1975504A (en) * | 1929-12-07 | 1934-10-02 | Richard Schreiber Gastell | Process and apparatus for preparing artificial threads |
| CN102061172A (en) * | 2010-11-19 | 2011-05-18 | 长春理工大学 | Europium (Eu) ion doped Y7O6F9 nanobelt and preparation method thereof |
| CN102060318A (en) * | 2010-11-19 | 2011-05-18 | 长春理工大学 | Terbium (Tb) doped Y7O6F9 nanobelt and preparation method thereof |
| CN102605471A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Method for preparing Tb (terbium)-doped sodium yttrium tetrafluoride green luminescent nanometer fiber |
-
2012
- 2012-08-10 CN CN201210283286.XA patent/CN102817113B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1975504A (en) * | 1929-12-07 | 1934-10-02 | Richard Schreiber Gastell | Process and apparatus for preparing artificial threads |
| CN102061172A (en) * | 2010-11-19 | 2011-05-18 | 长春理工大学 | Europium (Eu) ion doped Y7O6F9 nanobelt and preparation method thereof |
| CN102060318A (en) * | 2010-11-19 | 2011-05-18 | 长春理工大学 | Terbium (Tb) doped Y7O6F9 nanobelt and preparation method thereof |
| CN102605471A (en) * | 2012-02-24 | 2012-07-25 | 长春理工大学 | Method for preparing Tb (terbium)-doped sodium yttrium tetrafluoride green luminescent nanometer fiber |
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