CN102660803A - Method for preparing europium-doped yttrium lithium tetrafluoride (YLF) nanobelt - Google Patents
Method for preparing europium-doped yttrium lithium tetrafluoride (YLF) nanobelt Download PDFInfo
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- CN102660803A CN102660803A CN2012100442173A CN201210044217A CN102660803A CN 102660803 A CN102660803 A CN 102660803A CN 2012100442173 A CN2012100442173 A CN 2012100442173A CN 201210044217 A CN201210044217 A CN 201210044217A CN 102660803 A CN102660803 A CN 102660803A
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Abstract
The invention relates to a method for preparing europium-doped yttrium lithium tetrafluoride (YLF) nanobelt, falling into the technical field of nanomaterial preparation. The method comprises the steps of preparing spinning solution; preparing PVP (polyvinyl pyrrolidone)/metal nitrate composite nanobelt by electrospinning method; preparing mixed oxide nanobelt; and preparing YLF:5%Eu<3+> nanobelt. The mixed oxide nanobelt is subjected to fluoride treatment with ammonium bifluoride by double-crucible method to obtain YLF:5%Eu<3+> red luminescent nanobelt, which has good crystallinity, width of 7.44+/-1.27 micrometer, thickness of 180 nm and length of above 100 micrometer. The YLF:5%Eu<3+> nanobelt is a novel red luminescent nanomaterial with important application value. The method is simple and feasible, can realize mass production, and has wide application prospect.
Description
Technical field
The present invention relates to the nano material preparation research field, relate to the method that europium tetrafluoro yttrium lithium nano belt is mixed in a kind of preparation specifically.
Background technology
The preparation of inorganic matter nano belt and property research are one of forward position focus of subject researchs such as material science, Condensed Matter Physics, chemistry at present.Nano belt is a kind of nano material that is banded structure of synthesizing with manual method, 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 owing to the performances such as novel structure and unique light, electricity, magnetic that it is different from pipe, wire material cause people's great attention.
The rare earth tetrafluoride is one of present efficient rare-earth ion doping luminous host owing to have abundant 4f energy level and lower phonon ability.Mix europium tetrafluoro yttrium lithium LiYF
4: Eu
3+Be a kind of important red illuminating material, have the important application prospect.Adopt methods such as the precipitation method, sol-gel process, microemulsion method, presoma pyrolysismethod, hydro-thermal and solvent-thermal method, polyalcohol method, higher boiling ligand solvent method, prepared LiYF
4: Eu
3+Nanocrystalline, nanometer rods, sheet, nano materials such as cube is nanocrystalline, hexahedron is nanocrystalline, octahedron is nanocrystalline, hollow tubular structures, nano wire, spindle.Mix europium tetrafluoro yttrium lithium LiYF
4: Eu
3+Nano belt is a kind of novel red luminescent material, will obtain important application in fields such as biomarker, false proof, luminous and demonstration, medical science detection, solar cell, chemistry and biology sensor, nano-devices, has broad application prospects.At present, do not see and mix europium tetrafluoro yttrium lithium LiYF
4: Eu
3+The report of nano belt.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning); This method is a kind of effective ways that prepare continuous, as to have macro length micro nanometer fiber, is at first proposed in 1934 by Formhals.This method mainly is used for preparing high polymer nanometer fiber; It is characterized in that making charged Polymer Solution or melt in electrostatic field, to receive the traction of electrostatic force and spray, invest the receiving screen on opposite, thereby realize wire drawing by nozzle; 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 inorganic compound such as oxidate nano fiber at the 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.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 metallo-organic compound 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).201010108039.7), titanium dioxide nano-belts (Chinese invention patent, grant number: ZL200810050948.2) and Gd employing electrostatic spinning techniques such as Dong Xiangting have prepared rare earth trifluoride nano belt (Chinese invention patent, application number:
3Ga
5O
12: Eu
3+Porous nano-belt (SCI, 2010,31 (7), 1291-1296).Do not see that at present adopting electrostatic spinning technique to combine with fluorination technology prepares LiYF
4: Eu
3+The report of emitting red light 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 Technology for Heating Processing all have material impact to the pattern and the size of final products.The present invention adopts electrostatic spinning technique earlier, with a hydronium(ion) oxidation lithium LiOHH
2O, yittrium oxide Y
2O
3With europium oxide Eu
2O
3Be raw material,, obtain lithium nitrate LiNO with evaporating behind the nitric acid dissolve
3, yttrium nitrate Y (NO
3)
3With europium nitrate Eu (NO
3)
3Mixed crystal adds solvent N, and dinethylformamide DMF and high polymer templates polyvinylpyrrolidone PVP obtain carrying out electrostatic spinning behind the spinning solution, under the experiment condition of the best, prepare PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band, it is heat-treated in air, obtain the mixed oxide nanoparticle band, adopt double crucible method, with ammonium acid fluoride NH
4HF
2Fluoridize for fluorization agent, prepared the LiYF of the pure phase of novel structure
4: Eu
3+The emitting red light nano belt.
Summary of the invention
Prior art adopts methods such as the precipitation method, sol-gel process, microemulsion method, presoma pyrolysismethod, hydro-thermal and solvent-thermal method, polyalcohol method, higher boiling ligand solvent method, has prepared LiYF
4: Eu
3+Nanocrystalline, nanometer rods, sheet, nano materials such as cube is nanocrystalline, hexahedron is nanocrystalline, octahedron is nanocrystalline, hollow tubular structures, nano wire, spindle.Use electrostatic spinning technique in the 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 trifluoride nano belt.For a kind of novel red Illuminant nanometer carrying material is provided in the nano belt field, we combine electrostatic spinning technique with fluorination technology, invented LiYF
4: Eu
3+The preparation method of emitting red light nano belt.
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/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band, it is heat-treated in air, obtained the mixed oxide nanoparticle band, adopt double crucible method, with ammonium acid fluoride NH
4HF
2Fluoridize for fluorization agent, prepared the LiYF of the pure phase of novel structure
4: Eu
3+The emitting red light nano belt.In the present invention, the mole percent of the europium ion of doping is 5%, is labeled as LiYF
4: 5%Eu
3+, i.e. that the present invention is prepared is LiYF
4: 5%Eu
3+The emitting red light nano belt.The steps include:
(1) preparing spinning solution
That use in lithium source, yttrium source and europium source is a hydronium(ion) oxidation lithium LiOHH
2O, yittrium oxide Y
2O
3With europium oxide Eu
2O
3, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 1300000, adopts N, and dinethylformamide DMF is a solvent, takes by weighing an a certain amount of hydronium(ion) oxidation lithium LiOHH
2O, yittrium oxide Y
2O
3With europium oxide Eu
2O
3, Li wherein
+, Y
3+And Eu
3+Mol ratio be 100: 95: 5, promptly the mole percent of europium ion is 5%, uses nitric acid HNO
3The evaporation of dissolving back obtains LiNO
3, Y (NO
3)
3And Eu (NO
3)
3Mixed crystal adds an amount of N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 5h in the room temperature lower magnetic force; And leave standstill 3h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 10%; PVP content 20%, solvent DMF content 70%;
(2) preparation PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band
The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm; The adjustment shower nozzle is vertical with horizontal plane, applies the DC voltage of 6kV, solidifies apart from 18cm; 20～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band;
(3) preparation mixed oxide nanoparticle band
With described PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains the mixed oxide nanoparticle band;
(4) preparation LiYF
4: 5%Eu
3+Nano belt
Fluorination reagent uses ammonium acid fluoride NH
4HF
2, adopt double crucible method, ammonium acid fluoride is put into monkey; Cover carbon-point above, described mixed oxide nanoparticle band is placed on above the carbon-point, monkey is put into bigger crucible; Between interior outer crucible, add excessive ammonium acid fluoride, add that on outer crucible the crucible lid puts into tube furnace, be warming up to 280 ℃ of insulation 2h with the heating rate of 2 ℃/min; Be warmed up to 500 ℃ of insulation 3h again; Rate of temperature fall with 1 ℃/min is cooled to 200 ℃ at last, naturally cools to room temperature with body of heater afterwards, obtains LiYF
4: 5%Eu
3+Emitting red light nano belt, width are 7.44 ± 1.27 μ m, and thickness is 180nm, and length is greater than 100 μ m.
At the LiYF described in the said process
4: 5%Eu
3+The emitting red light nano belt has good crystallinity, and the nano belt width is 7.44 ± 1.27 μ m, and thickness is 180nm, and length has realized goal of the invention greater than 100 μ m.
Description of drawings
Fig. 1 is LiYF
4: 5%Eu
3+The XRD spectra of nano belt;
Fig. 2 is LiYF
4: 5%Eu
3+The SEM photo of nano belt, this figure double as Figure of abstract;
Fig. 3 is LiYF
4: 5%Eu
3+The width distribution histogram of nano belt;
Fig. 4 is LiYF
4: 5%Eu
3+The EDS spectrogram of nano belt;
Fig. 5 is LiYF
4: 5%Eu
3+The exciting light spectrogram of nano belt;
Fig. 6 is LiYF
4: 5%Eu
3+The emission spectrum figure of nano belt.
The specific embodiment
The yittrium oxide Y that the present invention selected for use
2O
3With europium oxide Eu
2O
3Purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 1300000, N, dinethylformamide DMF, carbon-point, a hydronium(ion) oxidation lithium LiOHH
2O, ammonium acid fluoride NH
4HF
2With nitric acid HNO
3Be commercially available analysis net product; Used glass apparatus, crucible and equipment are instrument and equipments commonly used in the laboratory.
Embodiment: take by weighing an a certain amount of hydronium(ion) oxidation lithium LiOHH
2O, yittrium oxide Y
2O
3With europium oxide Eu
2O
3, Li wherein
+, Y
3+And Eu
3+Mol ratio be 100: 95: 5, promptly the mole percent of europium ion is 5%, uses nitric acid HNO
3The evaporation of dissolving back obtains LiNO
3, Y (NO
3)
3And Eu (NO
3)
3Mixed crystal adds an amount of N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 5h in the room temperature lower magnetic force; And leave standstill 3h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 10%; PVP content 20%, solvent DMF content 70%; The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm; The adjustment shower nozzle is vertical with horizontal plane, applies the DC voltage of 6kV, solidifies apart from 18cm; 20～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band; With described PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains the mixed oxide nanoparticle band; Fluorination reagent uses ammonium acid fluoride NH
4HF
2, adopt double crucible method, ammonium acid fluoride is put into monkey; Cover carbon-point above, described mixed oxide nanoparticle band is placed on above the carbon-point, monkey is put into bigger crucible; Between interior outer crucible, add excessive ammonium acid fluoride, add that on outer crucible the crucible lid puts into tube furnace, be warming up to 280 ℃ of insulation 2h with the heating rate of 2 ℃/min; Be warmed up to 500 ℃ of insulation 3h again; Rate of temperature fall with 1 ℃/min is cooled to 200 ℃ at last, naturally cools to room temperature with body of heater afterwards, obtains LiYF
4: 5%Eu
3+The emitting red light nano belt.Described LiYF
4: 5%Eu
3+Nano belt has good crystallinity, the d value of its diffraction maximum and relative intensity and LiYF
4The listed d value of PDF standard card (77-0816) consistent with relative intensity, belong to tetragonal crystal system, space group is I41/a, sees shown in Figure 1.Described LiYF
4: 5%Eu
3+Nano belt is nano strip, and thickness is 180nm, and length is seen shown in Figure 2 greater than 100 μ m.With the Shapiro-Wilk method to LiYF
4: 5%Eu
3+The width of nano belt carries out normal distribution-test, under 95% confidence level, and LiYF
4: 5%Eu
3+The width distribution of nano belt belongs to normal distribution, and width is 7.44 ± 1.27 μ m, sees shown in Figure 3.LiYF
4: 5%Eu
3+Nano belt is formed (the Au conductive layer of surface plating when Au derives from the SEM sample preparation, the Li element can not detect with the EDS spectrum) by Y, F and Eu element, sees shown in Figure 4.When the monitoring wavelength is 591nm, LiYF
4: 5%Eu
3+The strongest excitation peak of nano belt is positioned at the 395nm place, corresponding to Eu
3+ 7F
0→
5L
6Transition is seen shown in Figure 5.Under the ultraviolet excitation of 395nm, LiYF
4: 5%Eu
3+Nano belt is launched the bright red that main peak is positioned at 591nm and 614nm, corresponding to Eu
3+Ion
5D
0→
7F
1With
5D
0→
7F
2Transition, as shown in Figure 6.
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 (2)
1. one kind prepares the method for mixing europium tetrafluoro yttrium lithium nano belt, it is characterized in that the method that adopts electrostatic spinning technique to combine with fluorination technology; Use polyvinylpyrrolidone PVP to be high polymer templates; Adopt N, dinethylformamide DMF is a solvent, and fluorination reagent uses ammonium acid fluoride NH
4HF
2, the preparation product is europium ion-doped tetrafluoro yttrium lithium LiYF
4: Eu
3+The emitting red light nano belt the steps include:
(1) preparing spinning solution
That use in lithium source, yttrium source and europium source is a hydronium(ion) oxidation lithium LiOHH
2O, yittrium oxide Y
2O
3With europium oxide Eu
2O
3, high polymer templates adopts polyvinylpyrrolidone PVP, adopts N, and dinethylformamide DMF is a solvent, takes by weighing an a certain amount of hydronium(ion) oxidation lithium LiOHH
2O, yittrium oxide Y
2O
3With europium oxide Eu
2O
3, Li wherein
+, Y
3+And Eu
3+Mol ratio be 100: 95: 5, promptly the mole percent of europium ion is 5%, uses nitric acid HNO
3The evaporation of dissolving back obtains LiNO
3, Y (NO
3)
3And Eu (NO
3)
3Mixed crystal adds an amount of N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 5h in the room temperature lower magnetic force; And leave standstill 3h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 10%; PVP content 20%, solvent DMF content 70%;
(2) preparation PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band
The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm; The adjustment shower nozzle is vertical with horizontal plane, applies the DC voltage of 6kV, solidifies apart from 18cm; 20～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band;
(3) preparation mixed oxide nanoparticle band
With described PVP/ [LiNO
3+ Y (NO
3)
3+ Eu (NO
3)
3] the composite Nano band is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains the mixed oxide nanoparticle band;
(4) preparation LiYF
4: 5%Eu
3+Nano belt
Fluorination reagent uses ammonium acid fluoride NH
4HF
2, adopt double crucible method, ammonium acid fluoride is put into monkey; Cover carbon-point above, described mixed oxide nanoparticle band is placed on above the carbon-point, monkey is put into bigger crucible; Between interior outer crucible, add excessive ammonium acid fluoride, add that on outer crucible the crucible lid puts into tube furnace, be warming up to 280 ℃ of insulation 2h with the heating rate of 2 ℃/min; Be warmed up to 500 ℃ of insulation 3h again; Rate of temperature fall with 1 ℃/min is cooled to 200 ℃ at last, naturally cools to room temperature with body of heater afterwards, obtains LiYF
4: 5%Eu
3+Emitting red light nano belt, width are 7.44 ± 1.27 μ m, and thickness is 180nm, and length is greater than 100 μ m.
2. the method for europium tetrafluoro yttrium lithium nano belt is mixed in a kind of preparation according to claim 1, it is characterized in that, high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=1300000.
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| CN101798056A (en) * | 2010-02-10 | 2010-08-11 | 长春理工大学 | Rare earth fluoride nanobelt and preparation method thereof |
| CN102061172A (en) * | 2010-11-19 | 2011-05-18 | 长春理工大学 | Europium (Eu) ion doped Y7O6F9 nanobelt and preparation method thereof |
| CN102306775A (en) * | 2011-08-29 | 2012-01-04 | 长春理工大学 | Lithium iron phosphate nanobelt serving as cathode material of lithium ion battery and preparation method of lithium iron phosphate nanobelt |
-
2012
- 2012-02-24 CN CN201210044217.3A patent/CN102660803B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008057072A (en) * | 2006-08-31 | 2008-03-13 | Teijin Ltd | Rare earth metal element-containing crystalline metal oxide fiber and method for producing the same |
| CN101348951A (en) * | 2008-07-11 | 2009-01-21 | 长春理工大学 | Preparation of rare earth fluoride/rare earth oxyfluoride composite nano fibre |
| CN101798056A (en) * | 2010-02-10 | 2010-08-11 | 长春理工大学 | Rare earth fluoride nanobelt and preparation method thereof |
| CN102061172A (en) * | 2010-11-19 | 2011-05-18 | 长春理工大学 | Europium (Eu) ion doped Y7O6F9 nanobelt and preparation method thereof |
| CN102306775A (en) * | 2011-08-29 | 2012-01-04 | 长春理工大学 | Lithium iron phosphate nanobelt serving as cathode material of lithium ion battery and preparation method of lithium iron phosphate nanobelt |
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