CN102660807B - 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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CN102660807B
CN102660807B CN201210044545.3A CN201210044545A CN102660807B CN 102660807 B CN102660807 B CN 102660807B CN 201210044545 A CN201210044545 A CN 201210044545A CN 102660807 B CN102660807 B CN 102660807B
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conversion luminescence
nanobelt
ytterbium
pvp
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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 nanobelt of a kind of erbium ytterbium
Technical field
The present invention relates to nano material preparation research field, relate to specifically the two preparation methods that mix tetrafluoro yttrium sodium up-conversion luminescence nanobelt of a kind of erbium ytterbium.
Background technology
The preparation of inorganic matter nanobelt and property research are one of forward position focus of the subject researchs such as material science, Condensed Matter Physics, chemistry at present.Nanobelt is a kind of nano material that is banded structure of synthesizing by artificial means, 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 hundreds of micron, even several millimeters.Nanobelt is different from the performances such as the novel structure of pipe, wire material and unique optical, electrical, magnetic and causes people's great attention due to it.
Up-conversion luminescence process refers to that material absorbs the process of sending higher-energy photon compared with energy photons, and this special nature that up-conversion has makes it in laser technology, optical fiber communication technology, fibre amplifier, Display Technique and the numerous areas such as false proof, have broad application prospects.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, upper 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 conventionally 3+for sensitizer.Rare earth tetrafluoride, owing to having abundant 4f energy level and lower phonon energy, is one of matrix of current 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, there is important application prospect.Adopt the 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+the nano materials such as nanocrystalline, nanometer rods, sheet, cube is nanocrystalline, hexahedron is nanocrystalline, octahedra nanocrystalline, hollow tubular structures, nano wire, spindle.The two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+up-conversion luminescence nanobelt 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, have no the two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+the report of up-conversion luminescence nanobelt.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning), the method is to prepare a kind of effective ways of continuous, to have macro length micro nanometer fiber, by Formhals, in 1934, is first proposed.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, at inorfil preparing technical field, occurred adopting electrospinning process to prepare inorganic compound as the technical scheme of oxidate nano fiber, 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 and prepared porous SnO with metallo-organic compound decomposition technique 2nanobelt (Nanotechnology, 2007,18:435704); Someone utilizes electrostatic spinning technique first to prepare PEO/ stannic hydroxide composite Nano band, and its roasting has been obtained to porous SnO 2nanobelt (J.Am.Ceram.Soc., 2008,91 (1): 257-262).201010108039.7), titanium dioxide nano-belts (Chinese invention patent, grant number: ZL200810050948.2) and Gd the employing electrostatic spinning techniques such as Dong Xiangting have been prepared trifluorides nanobelt (Chinese invention patent, application number: 3ga 5o 12: Eu 3+porous nano-belt (SCI, 2010,31 (7), 1291-1296).Have no at present and adopt electrostatic spinning technique to combine with fluorination technology to prepare NaYF 4: Er 3+, Yb 3+the report of up-conversion luminescence nanobelt.
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 have material impact to the pattern of final products and size.The present invention first adopts electrostatic spinning technique, with sodium carbonate Na 2cO 3, yittrium oxide Y 2o 3, erbium oxide Er 2o 3with ytterbium oxide Yb 2o 3for raw material, with evaporating after nitric acid dissolve, obtain sodium nitrate NaNO 3, yttrium nitrate Y (NO 3) 3, erbium nitrate Er (NO 3) 3with ytterbium nitrate Yb (NO 3) 3mixed crystal, adds solvent DMF DMF and high polymer templates polyvinylpyrrolidone PVP, obtains carrying out electrostatic spinning after spinning solution, under best experiment condition, prepares PVP/[NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] composite Nano band, it is heat-treated in air, obtain mixed oxide nanoparticle band, adopt double crucible method, with ammonium acid fluoride NH 4hF 2for fluorization agent, fluoridize, prepared the NaYF of novel structure pure phase 4: Er 3+, Yb 3+up-conversion luminescence nanobelt.
Summary of the invention
Prior art adopts the 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+the nano materials such as nanocrystalline, nanometer rods, sheet, cube is nanocrystalline, hexahedron is nanocrystalline, octahedra nanocrystalline, hollow tubular structures, nano wire, spindle.Use electrostatic spinning technique in background technology has been prepared metal oxide, composite oxide of metal nanofiber, high molecular nanometer band, SnO 2nanobelt, TiO 2nanobelt, Gd 3ga 5o 12: Eu 3+porous nano-belt and trifluorides nanobelt.For a kind of novel up-conversion luminescence nanobelt material is provided in nanobelt field, we combine electrostatic spinning technique with fluorination technology, invented NaYF 4: Er 3+, Yb 3+the preparation method of up-conversion luminescence nanobelt.
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/[NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] composite Nano band, it is heat-treated in air, obtained mixed oxide nanoparticle band, adopt double crucible method, with ammonium acid fluoride NH 4hF 2for fluorization agent, fluoridize, prepared the NaYF of novel structure pure phase 4: Er 3+, Yb 3+up-conversion luminescence nanobelt.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) preparation spinning solution
That He Yi source, ,Er source, ,Yi source, sodium source is used 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, and adopting DMF DMF is solvent, takes 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 3after dissolving, evaporation, obtains NaNO 3, Y (NO 3) 3, Er (NO 3) 3and Yb (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 8h, and standing 6h, 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] composite Nano band
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, adjust shower nozzle vertical with horizontal plane, apply the DC voltage of 6kV, solidify 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] composite Nano band;
(3) prepare mixed oxide nanoparticle band
By described PVP/[NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] composite Nano band is put in temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle band;
(4) prepare NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt
Fluorination reagent is used ammonium acid fluoride NH 4hF 2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle band is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add excessive ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, then is warmed up to 500 ℃ of insulation 3h, and finally the rate of temperature fall with 1 ℃/min is cooled to 200 ℃, with body of heater, naturally cool to room temperature afterwards, obtain NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt, nanobelt width is 3.04 ± 0.52 μ m, and thickness is 112nm, and length is greater than 50 μ m.
At the NaYF described in said process 4: Er 3+, Yb 3+up-conversion luminescence nanobelt has good crystallinity, and nanobelt width is 3.04 ± 0.52 μ m, and thickness is 112nm, and length is greater than 50 μ m, has realized goal of the invention.
Accompanying drawing explanation
Fig. 1 is NaYF 4: Er 3+, Yb 3+the XRD spectra of up-conversion luminescence nanobelt;
Fig. 2 is NaYF 4: Er 3+, Yb 3+the SEM photo of up-conversion luminescence nanobelt, this figure doubles as Figure of abstract;
Fig. 3 is NaYF 4: Er 3+, Yb 3+the width distribution histogram of up-conversion luminescence nanobelt;
Fig. 4 is NaYF 4: Er 3+, Yb 3+the EDS spectrogram of up-conversion luminescence nanobelt;
Fig. 5 is NaYF 4: Er 3+, Yb 3+the upper switching emission spectrogram of up-conversion luminescence nanobelt;
Fig. 6 is NaYF 4: Er 3+, Yb 3+the upper switching emission spectrogram of up-conversion luminescence nanobelt when the diode laser of different exciting powers excites;
Fig. 7 is NaYF 4: Er 3+, Yb 3+two natural logrithm figure between the Up-conversion Intensity of up-conversion luminescence nanobelt and the exciting power of diode laser.
The specific embodiment
The yittrium oxide Y that the present invention is selected 2o 3, erbium oxide Er 2o 3with ytterbium oxide Yb 2o 3purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 1300000, DMF DMF, carbon-point, sodium carbonate Na 2cO 3, ammonium acid fluoride NH 4hF 2with nitric acid HNO 3be commercially available analysis net product; Glass apparatus used, crucible and equipment are instrument and equipments conventional in laboratory.
Embodiment: take 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 3after dissolving, evaporation, obtains NaNO 3, Y (NO 3) 3, Er (NO 3) 3and Yb (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 8h, and standing 6h, 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 preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, adjust shower nozzle vertical with horizontal plane, apply the DC voltage of 6kV, solidify 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] composite Nano band; By described PVP/[NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] composite Nano band is put in temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle band; Fluorination reagent is used ammonium acid fluoride NH 4hF 2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle band is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add excessive ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, then is warmed up to 500 ℃ of insulation 3h, and finally the rate of temperature fall with 1 ℃/min is cooled to 200 ℃, with body of heater, naturally cool to room temperature afterwards, obtain NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt.Described NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt, 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, as shown in Figure 1.Described NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt is nano strip, and thickness is 112nm, and length is greater than 50 μ m, as shown in Figure 2.By Shapiro-Wilk method to NaYF 4: Er 3+, Yb 3+the width of up-conversion luminescence nanobelt carries out normal distribution-test, under 95% confidence level, and NaYF 4: Er 3+, Yb 3+the width distribution of up-conversion luminescence nanobelt belongs to normal distribution, and width is 3.04 ± 0.52 μ m, as shown in Figure 3.NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt forms (the Au conductive layer of plated surface when Au derives from SEM sample preparation) by Na, Y, F, Er and Yb element, as shown in Figure 4.With wavelength be the diode laser of 980nm, power 269mW as excitation source, obtain NaYF 4: Er 3+, Yb 3+the upper switching emission spectrum of up-conversion luminescence nanobelt, the bands of a spectrum that are respectively 407nm, 519nm, 538nm and 651nm by peak value form, wherein the corresponding Er of the blue emission at 407nm place 3+ion 2h 9/2→ 4i 15/2transition transmitting, the corresponding Er of green emission at 519nm and 538nm place 3+ion 2h 11/2→ 4i 15/2with 4s 3/2→ 4i 15/2transition transmitting, and the corresponding Er of the red emission at 651nm place 3+ion 4f 9/2→ 4i 15/2transition transmitting, as shown in Figure 5.NaYF 4: Er 3+, Yb 3+the upper switching emission spectrum of up-conversion luminescence nanobelt strengthens along with the increase of the exciting power of diode laser, as shown in Figure 6.By NaYF 4: Er 3+, Yb 3+green emission in the upper switching emission spectrum of up-conversion luminescence nanobelt 4s 3/2→ 4i 15/2transition and red emission 4f 9/2→ 4i 15/2the natural logrithm lnP mapping of the natural logrithm lnI of the Up-conversion Intensity of transition to the exciting power of diode laser, obtains two straight lines, wherein 4s 3/2→ 4i 15/2transition and 4f 9/2→ 4i 15/2the slope n of transition is respectively 3.337 and 3.7903, shows green emission 4s 3/2→ 4i 15/2for three-photon process, red emission 4f 9/2→ 4i 15/2be four photon process, as shown in Figure 7.
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. two preparation methods that mix tetrafluoro yttrium sodium up-conversion luminescence nanobelt of an erbium ytterbium, 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=1300000 is high polymer templates, adopt N, dinethylformamide DMF is solvent, and fluorination reagent is used ammonium acid fluoride NH 4hF 2, preparing product is the two tetrafluoro yttrium sodium NaYF that mix of erbium ytterbium 4: Er 3+, Yb 3+up-conversion luminescence nanobelt, the steps include:
(1) preparation spinning solution
That He Yi source, ,Er source, ,Yi source, sodium source is used 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 adopting DMF DMF is solvent, takes 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 3after dissolving, evaporation, obtains NaNO 3, Y (NO 3) 3, Er (NO 3) 3and Yb (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 8h, and standing 6h, 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] composite Nano band
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, adjust shower nozzle vertical with horizontal plane, apply the DC voltage of 6kV, solidify 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] composite Nano band;
(3) prepare mixed oxide nanoparticle band
By described PVP/[NaNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] composite Nano band is put in temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle band;
(4) prepare NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt
Fluorination reagent is used ammonium acid fluoride NH 4hF 2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle band is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add excessive ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, then is warmed up to 500 ℃ of insulation 3h, and finally the rate of temperature fall with 1 ℃/min is cooled to 200 ℃, with body of heater, naturally cool to room temperature afterwards, obtain NaYF 4: Er 3+, Yb 3+up-conversion luminescence nanobelt, width is 3.04 ± 0.52 μ m, and thickness is 112nm, and length is greater than 50 μ m.
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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