CN102660807A - Method for preparing erbium/ytterbium co-doped NaYF4 up-conversion luminescence nanometer belt - Google Patents

Method for preparing erbium/ytterbium co-doped NaYF4 up-conversion luminescence nanometer belt Download PDF

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CN102660807A
CN102660807A CN2012100445453A CN201210044545A CN102660807A CN 102660807 A CN102660807 A CN 102660807A CN 2012100445453 A CN2012100445453 A CN 2012100445453A CN 201210044545 A CN201210044545 A CN 201210044545A CN 102660807 A CN102660807 A CN 102660807A
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nano
conversion luminescence
ytterbium
erbium
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CN102660807B (en
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董相廷
于飞
于文生
王进贤
刘桂霞
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Changchun University of Science and Technology
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Abstract

The present invention relates to a method for preparing an erbium/ytterbium co-doped NaYF4 up-conversion luminescence nanometer belt, belonging to the technical field of nano material preparation. The method comprises the following four steps: (1) preparing a spinning solution; (2) preparing a PVP/metal nitrate composite nanometer belt by using an electrospinning technology; (3) preparing a mixed oxide nanometer belt; and (4) preparing a NaYF4: Er<3+>,Yb<3+> up-conversion luminescence nanometer belt. By adopting a double crucible method, a fluorination treatment is applied on the mixed oxide nanometer belt by using ammonium acid fluoride to obtain the NaYF4: Er<3+>,Yb<3+> up-conversion luminescence nanometer belt with good crystallization, width being the result of 3.04+-0.52 mum, thickness being 112 nanometers and length being greater than 50 micrometers. The up-conversion luminescence nanometer belt is a nanometer luminescence material with an important application value. The preparation method provided in the invention is characterized by simple operation, and is capable of mass production, being provided with a wide application prospect.

Description

The two preparation methods that mix tetrafluoro yttrium sodium up-conversion luminescence nano belt of a kind of erbium ytterbium
Technical field
The present invention relates to the nano material preparation research field, relate to the two preparation methods that mix tetrafluoro yttrium sodium up-conversion luminescence nano belt of a kind of erbium ytterbium 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 up-conversion luminescence process is meant that absorbed sends the process of higher-energy photon than energy photons, and this special nature that up-conversion had makes it have broad application prospects in laser technology, optical fiber communication technology, fibre amplifier, Display Technique and numerous areas such as false proof.Up-conversion generally includes activator, sensitizer and matrix.Erbium ion Er 3+Have abundant energy level, and part is longer the life time of the level, last conversion efficiency is very high, is the activator of the more up-conversion of research at present.With Er 3+Ion is that the up-conversion of activator adopts ytterbium ion Yb usually 3+Be sensitizer.The rare earth tetrafluoride because have abundant 4f energy level and lower phonon can, be one of matrix of at present rare earth ion doped efficient up-conversion luminescent material.The two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+Be a kind of important up-conversion luminescent material, have the important application prospect.Adopt methods such as microemulsion method, presoma pyrolysismethod, hydro-thermal and solvent-thermal method, the precipitation method, sol-gel process, polyalcohol method, higher boiling ligand solvent method, prepared NaYF 4: Er 3+, Yb 3+Nanocrystalline, nanometer rods, sheet, nano materials such as cube is nanocrystalline, hexahedron is nanocrystalline, octahedron is nanocrystalline, hollow tubular structures, nano wire, spindle.The two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+The up-conversion luminescence nano belt is a kind of novel 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, do not see the two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+The report of up-conversion luminescence 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 NaYF 4: Er 3+, Yb 3+The report of up-conversion luminescence 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 sodium carbonate Na 2CO 3, yittrium oxide Y 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3Be raw material,, obtain sodium nitrate NaNO with evaporating behind the nitric acid dissolve 3, yttrium nitrate Y (NO 3) 3, erbium nitrate Er (NO 3) 3With ytterbium nitrate Yb (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/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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 NaYF of the pure phase of novel structure 4: Er 3+, Yb 3+The up-conversion luminescence nano belt.
Summary of the invention
Prior art adopts methods such as microemulsion method, presoma pyrolysismethod, hydro-thermal and solvent-thermal method, the precipitation method, sol-gel process, polyalcohol method, higher boiling ligand solvent method, has prepared NaYF 4: Er 3+, Yb 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 up-conversion luminescence nano belt material is provided in the nano belt field, we combine electrostatic spinning technique with fluorination technology, invented NaYF 4: Er 3+, Yb 3+The preparation method of up-conversion luminescence 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/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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 NaYF of the pure phase of novel structure 4: Er 3+, Yb 3+The up-conversion luminescence nano belt.In the present invention, the erbium ion Er of doping 3+With ytterbium ion Yb 3+Mole percent be respectively 1% and 20%.The steps include:
(1) preparing spinning solution
That use in sodium source, yttrium source, erbium source and ytterbium source is sodium carbonate Na 2CO 3, yittrium oxide Y 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 1300000, adopts N, and dinethylformamide DMF is a solvent, takes by weighing a certain amount of sodium carbonate Na 2CO 3, yittrium oxide Y 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3, Na wherein +, Y 3+, Er 3+And Yb 3+Mol ratio be 100: 79: 1: 20, i.e. erbium ion Er 3+With ytterbium ion Yb 3+Mole percent be 1% and 20%, use nitric acid HNO 3The evaporation of dissolving back obtains NaNO 3, Y (NO 3) 3, Er (NO 3) 3And Yb (NO 3) 3Mixed crystal adds an amount of N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 8h in the room temperature lower magnetic force; And leave standstill 6h, 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) PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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; 18～28 ℃ of room temperatures, relative humidity is 55%～70%, obtains PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band;
(3) preparation mixed oxide nanoparticle band
With described PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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 NaYF 4: Er 3+, Yb 3+The up-conversion luminescence 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 NaYF 4: Er 3+, Yb 3+Up-conversion luminescence nano belt, nano belt width are 3.04 ± 0.52 μ m, and thickness is 112nm, and length is greater than 50 μ m.
At the NaYF described in the said process 4: Er 3+, Yb 3+The up-conversion luminescence nano belt has good crystallinity, and the nano belt width is 3.04 ± 0.52 μ m, and thickness is 112nm, and length has realized goal of the invention greater than 50 μ m.
Description of drawings
Fig. 1 is NaYF 4: Er 3+, Yb 3+The XRD spectra of up-conversion luminescence nano belt;
Fig. 2 is NaYF 4: Er 3+, Yb 3+The SEM photo of up-conversion luminescence nano belt, this figure double as Figure of abstract;
Fig. 3 is NaYF 4: Er 3+, Yb 3+The width distribution histogram of up-conversion luminescence nano belt;
Fig. 4 is NaYF 4: Er 3+, Yb 3+The EDS spectrogram of up-conversion luminescence nano belt;
Fig. 5 is NaYF 4: Er 3+, Yb 3+The last switching emission spectrogram of up-conversion luminescence nano belt;
Fig. 6 is NaYF 4: Er 3+, Yb 3+The up-conversion luminescence nano belt when the diode laser of different exciting powers excites on the switching emission spectrogram;
Fig. 7 is NaYF 4: Er 3+, Yb 3+Two natural logrithm figure between the up-conversion luminescence intensity of up-conversion luminescence nano belt and the exciting power of diode laser.
The specific embodiment
The yittrium oxide Y that the present invention selected for use 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3Purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 1300000, N, dinethylformamide DMF, carbon-point, sodium carbonate Na 2CO 3, 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 a certain amount of sodium carbonate Na 2CO 3, yittrium oxide Y 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3, Na wherein +, Y 3+, Er 3+And Yb 3+Mol ratio be 100: 79: 1: 20, i.e. erbium ion Er 3+With ytterbium ion Yb 3+Mole percent be 1% and 20%, use nitric acid HNO 3The evaporation of dissolving back obtains NaNO 3, Y (NO 3) 3, Er (NO 3) 3And Yb (NO 3) 3Mixed crystal adds an amount of N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 8h in the room temperature lower magnetic force; And leave standstill 6h, 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; 18～28 ℃ of room temperatures, relative humidity is 55%～70%, obtains PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band; With described PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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 NaYF 4: Er 3+, Yb 3+The up-conversion luminescence nano belt.Described NaYF 4: Er 3+, Yb 3+The up-conversion luminescence nano belt has good crystallinity, the d value of its diffraction maximum and relative intensity and NaYF 4The listed d value of PDF standard card (16-0334) consistent with relative intensity, belong to hexagonal crystal system, space group is P63/m, sees shown in Figure 1.Described NaYF 4: Er 3+, Yb 3+The up-conversion luminescence nano belt is nano strip, and thickness is 112nm, and length is seen shown in Figure 2 greater than 50 μ m.With the Shapiro-Wilk method to NaYF 4: Er 3+, Yb 3+The width of up-conversion luminescence nano belt carries out normal distribution-test, under 95% confidence level, and NaYF 4: Er 3+, Yb 3+The width distribution of up-conversion luminescence nano belt belongs to normal distribution, and width is 3.04 ± 0.52 μ m, sees shown in Figure 3.NaYF 4: Er 3+, Yb 3+The up-conversion luminescence nano belt is formed (the Au conductive layer of surface plating when Au derives from the SEM sample preparation) by Na, Y, F, Er and Yb element, sees shown in Figure 4.Use wavelength as the diode laser of 980nm, power 269mW as excitation source, obtain NaYF 4: Er 3+, Yb 3+The last switching emission spectrum of up-conversion luminescence nano belt, the bands of a spectrum that are respectively 407nm, 519nm, 538nm and 651nm by peak value are formed, wherein the corresponding Er of the blue emission at 407nm place 3+Ion 2H 9/2→ 4I 15/2The transition emission, the corresponding Er of the green emission at 519nm and 538nm place 3+Ion 2H 11/2→ 4I 15/2With 4S 3/2→ 4I 15/2Transition emission, and the corresponding Er of the red emission at 651nm place 3+Ion 4F 9/2→ 4I 15/2The transition emission is seen shown in Figure 5.NaYF 4: Er 3+, Yb 3+The last switching emission spectrum of up-conversion luminescence nano belt strengthens along with the increase of the exciting power of diode laser, sees shown in Figure 6.With NaYF 4: Er 3+, Yb 3+Green emission in the last switching emission spectrum of up-conversion luminescence nano belt 4S 3/2→ 4I 15/2Transition and red emission 4F 9/2→ 4I 15/2The natural logrithm lnI of the up-conversion luminescence intensity of transition obtains two straight lines, wherein to the natural logrithm lnP mapping of the exciting power of diode laser 4S 3/2→ 4I 15/2Transition with 4F 9/2→ 4I 15/2The slope n of transition is respectively 3.337 and 3.7903, shows green emission 4S 3/2→ 4I 15/2Be three-photon process, red emission 4F 9/2→ 4I 15/2Be four photon process, see shown in Figure 7.
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. two preparation methods that mix tetrafluoro yttrium sodium up-conversion luminescence nano belt of an erbium ytterbium; It is characterized in that; The method that adopts electrostatic spinning technique to combine with fluorination technology uses polyvinylpyrrolidone PVP to be high polymer templates, adopts N; Dinethylformamide DMF is a solvent, and fluorination reagent uses ammonium acid fluoride NH 4HF 2, the preparation product is the two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+The up-conversion luminescence nano belt the steps include:
(1) preparing spinning solution
That use in sodium source, yttrium source, erbium source and ytterbium source is sodium carbonate Na 2CO 3, yittrium oxide Y 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3, high polymer templates adopts polyvinylpyrrolidone PVP, adopts N, and dinethylformamide DMF is a solvent, takes by weighing a certain amount of sodium carbonate Na 2CO 3, yittrium oxide Y 2O 3, erbium oxide Er 2O 3With ytterbium oxide Yb 2O 3, Na wherein +, Y3 +, Er 3+And Yb 3+Mol ratio be 100: 79: 1: 20, i.e. erbium ion Er 3+With ytterbium ion Yb 3+Mole percent be 1% and 20%, use nitric acid HNO 3The evaporation of dissolving back obtains NaNO 3, Y (NO 3) 3, Er (NO 3) 3And Yb (NO 3) 3Mixed crystal adds an amount of N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 8h in the room temperature lower magnetic force; And leave standstill 6h, 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) PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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; 18～28 ℃ of room temperatures, relative humidity is 55%～70%, obtains PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band;
(3) preparation mixed oxide nanoparticle band
With described PVP/ [NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (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 NaYF 4: Er 3+, Yb 3+The up-conversion luminescence 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 NaYF 4: Er 3+, Yb 3+Up-conversion luminescence nano belt, width are 3.04 ± 0.52 μ m, and thickness is 112nm, and length is greater than 50 μ m.
2. the two preparation methods that mix tetrafluoro yttrium sodium up-conversion luminescence nano belt of a kind of erbium ytterbium according to claim 1 is characterized in that high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=1300000.
CN201210044545.3A 2012-02-24 2012-02-24 Method for preparing erbium/ytterbium co-doped NaYF4 up-conversion luminescence nanometer belt Expired - Fee Related CN102660807B (en)

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