CN102660801B - Method for preparing erbium and ytterbium double-doped yttrium lithium tetrafluoride up-conversion luminescent nanobelt - Google Patents

Method for preparing erbium and ytterbium double-doped yttrium lithium tetrafluoride up-conversion luminescent nanobelt Download PDF

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CN102660801B
CN102660801B CN 201210044190 CN201210044190A CN102660801B CN 102660801 B CN102660801 B CN 102660801B CN 201210044190 CN201210044190 CN 201210044190 CN 201210044190 A CN201210044190 A CN 201210044190A CN 102660801 B CN102660801 B CN 102660801B
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nanobelt
pvp
erbium
ytterbium
oxide
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CN102660801A (en
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王进贤
董相廷
于飞
于文生
刘桂霞
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Changchun University of Science and Technology
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Abstract

The invention relates to a preparation method for an erbium and ytterbium double-doped up-conversion luminescent nanobelt and belongs to the field of nano-material preparation, comprising the four steps of (1) preparing a spinning solution; (2) preparing a PVP/metal nitrate composite nanobelt using a static spinning technique; (3) preparing a mixed oxide nanobelt; and (4) preparing a LiYF4:Er3+, Yb3+ up-conversion luminescent nanobelt. Fluorination of the mixed oxide nanobelt with ammonium bifluoride by a double-crucible method is performed, and the LiYF4:Er3+, Yb3+ up-conversion luminescent nanobelt having a width of 7.79+/-0.32[mu]m, a thickness of 69.1nm and a length greater than 50 [mu]m with good crystallinity is obtained. The up-conversion luminescent nanobelt is a nano luminescent material having significant application value. The preparation method is simple to operate and suitable for mass production, having a broad application prospect.

Description

A kind of two methods of mixing tetrafluoro yttrium lithium up-conversion luminescence nanobelt of erbium ytterbium that prepare
Technical field
The present invention relates to nano material preparation research field, relate to specifically a kind of two methods of mixing tetrafluoro yttrium lithium up-conversion luminescence nanobelt of erbium ytterbium that prepare.
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 the hundreds of micron, even several millimeters.Nanobelt is different from the performances such as the novel structure of pipe, wire material and unique light, electricity, magnetic and causes people's great attention due to it.
The up-conversion luminescence process refers to that material absorbs the process of sending the higher-energy photon than energy photons, and this special nature that up-conversion has makes it have broad application prospects in laser technology, optical fiber communication technology, fibre amplifier, Display Technique and the 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, upper conversion efficiency is very high, is the activator of the more up-conversion of research at present.With Er 3+the up-conversion that ion is activator adopts ytterbium ion Yb usually 3+for sensitizer.The rare earth tetrafluoride is owing to having abundant 4f energy level and lower phonon energy, is one of matrix of at present rare earth ion doped efficient up-conversion luminescent material.The two tetrafluoro yttrium lithium LiYF that mix of erbium ytterbium 4: Er 3+, Yb 3+be a kind of important up-conversion luminescent material, there is the 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 LiYF 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 lithium LiYF that mix of erbium ytterbium 4: Er 3+, Yb 3+the 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 lithium LiYF that mix of erbium ytterbium 4: Er 3+, Yb 3+the report of up-conversion luminescence nanobelt.
The United States Patent (USP) that the patent No. is 1975504 discloses the technical scheme of a relevant electrospinning process (electrospinning), the method is a kind of effective ways that prepare continuous, as to have macro length micro nanometer fiber, by Formhals, in 1934, is at first proposed.This method is mainly used to prepare high polymer nanometer fiber, it is characterized in that making charged Polymer Solution or melt are subject to the traction of electrostatic force and are sprayed by nozzle in electrostatic field, 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 the inorfil preparing technical field, occurred adopting electrospinning process to prepare the technical scheme of inorganic compound as the 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 the metallo-organic compound decomposition technique 2nanobelt (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 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 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 LiYF 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 pattern and the size of final products.The present invention first adopts electrostatic spinning technique, with a hydronium(ion) oxidation lithium LiOHH 2o, yittrium oxide Y 2o 3, erbium oxide Er 2o 3with ytterbium oxide Yb 2o 3for raw material, with evaporating after nitric acid dissolve, obtain lithium nitrate LiNO 3, yttrium nitrate Y (NO 3) 3, erbium nitrate Er (NO 3) 3with ytterbium nitrate Yb (NO 3) 3mixed crystal, add solvent DMF DMF and high polymer templates polyvinylpyrrolidone PVP, obtains carrying out electrostatic spinning after spinning solution, under best experiment condition, prepares PVP/[LiNO 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 2fluoridized for fluorization agent, prepared the LiYF of novel structure pure phase 4: Er 3+, Yb 3+the 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 LiYF 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 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 the nanobelt field, we combine electrostatic spinning technique with fluorination technology, invented LiYF 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 at first preparing for electrostatic spinning, and the application electrostatic spinning technique carries out electrostatic spinning, under best experiment condition, prepares PVP/[LiNO 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 2fluoridized for fluorization agent, prepared the LiYF of novel structure pure phase 4: Er 3+, Yb 3+the 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, lithium source is used is a hydronium(ion) oxidation lithium LiOHH 2o, 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 an a certain amount of hydronium(ion) oxidation lithium LiOHH 2o, yittrium oxide Y 2o 3, erbium oxide Er 2o 3with ytterbium oxide Yb 2o 3, Li 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, obtain LiNO 3, Y (NO 3) 3, Er (NO 3) 3and Yb (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, stir 6h in the room temperature lower magnetic force, and standing 4h, 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/[LiNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band
The spinning solution prepared 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, 20～28 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/[LiNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band;
(3) prepare the mixed oxide nanoparticle band
By described PVP/[LiNO 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, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature with body of heater afterwards, obtains the mixed oxide nanoparticle band;
(4) prepare LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt
Fluorination reagent is used ammonium acid fluoride NH 4hF 2adopt double crucible method, ammonium acid fluoride is put into to monkey, the above covers carbon-point, described mixed oxide nanoparticle band is placed on above carbon-point, monkey is put into to larger crucible, add excessive ammonium acid fluoride between interior outer crucible, add that on outer crucible the 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 ℃, naturally cool to room temperature with body of heater afterwards, obtain LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt, width is 7.97 ± 0.32 μ m, and thickness is 69.1nm, and length is greater than 50 μ m.
At the LiYF described in said process 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt has good crystallinity, and the nanobelt width is 7.97 ± 0.32 μ m, and thickness is 69.1nm, and length is greater than 50 μ m, has realized goal of the invention.
The accompanying drawing explanation
Fig. 1 is LiYF 4: Er 3+, Yb 3+the XRD spectra of up-conversion luminescence nanobelt;
Fig. 2 is LiYF 4: Er 3+, Yb 3+the SEM photo of up-conversion luminescence nanobelt, this figure doubles as Figure of abstract;
Fig. 3 is LiYF 4: Er 3+, Yb 3+the width distribution histogram of up-conversion luminescence nanobelt;
Fig. 4 is LiYF 4: Er 3+, Yb 3+the EDS spectrogram of up-conversion luminescence nanobelt;
Fig. 5 is LiYF 4: Er 3+, Yb 3+the upper switching emission spectrogram of up-conversion luminescence nanobelt;
Fig. 6 is LiYF 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 LiYF 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, a hydronium(ion) oxidation lithium LiOHH 2o, 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 commonly used in laboratory.
Embodiment: take an a certain amount of hydronium(ion) oxidation lithium LiOHH 2o, yittrium oxide Y 2o 3, erbium oxide Er 2o 3with ytterbium oxide Yb 2o 3, Li 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, obtain LiNO 3, Y (NO 3) 3, Er (NO 3) 3and Yb (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, stir 6h in the room temperature lower magnetic force, and standing 4h, 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 prepared 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, 20～28 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/[LiNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band; By described PVP/[LiNO 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, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature with body of heater afterwards, obtains the mixed oxide nanoparticle band; Fluorination reagent is used ammonium acid fluoride NH 4hF 2adopt double crucible method, ammonium acid fluoride is put into to monkey, the above covers carbon-point, described mixed oxide nanoparticle band is placed on above carbon-point, monkey is put into to larger crucible, add excessive ammonium acid fluoride between interior outer crucible, add that on outer crucible the 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 ℃, naturally cool to room temperature with body of heater afterwards, obtain LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt.Described LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt, have 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, as shown in Figure 1.Described LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt is nano strip, and thickness is 69.1nm, and length is greater than 50 μ m, as shown in Figure 2.By the Shapiro-Wilk method to LiYF 4: Er 3+, Yb 3+the width of up-conversion luminescence nanobelt carries out normal distribution-test, under 95% confidence level, and LiYF 4: Er 3+, Yb 3+the width distribution of up-conversion luminescence nanobelt belongs to normal distribution, and width is 7.97 ± 0.32 μ m, as shown in Figure 3.LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt forms (the Au conductive layer of plated surface when Au derives from the SEM sample preparation, the Li element can not detect by the EDS spectrum) by Y, F, Er and Yb element, as shown in Figure 4.The diode laser that is 980nm, power 549mW with wavelength, as excitation source, obtains LiYF 4: Er 3+, Yb 3+the upper switching emission spectrum of up-conversion luminescence nanobelt, the bands of a spectrum that are respectively 407nm, 520nm, 548nm and 650nm by peak value form, 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 520nm and 548nm 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 650nm place 3+ion 4f 9/2→ 4i 15/2the transition emission, as shown in Figure 5.LiYF 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 LiYF 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, obtain two straight lines, wherein 4s 3/2→ 4i 15/2transition and 4f 9/2→ 4i 15/2the slope n of transition is respectively 2.7130 and 2.8507, shows green emission 4s 3/2→ 4i 15/2and red emission 4f 9/2→ 4i 15/2be the three-photon process, as shown in Figure 7.
Certainly; the present invention also can have other various embodiments; in the situation that do not deviate 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. one kind prepares the two methods of mixing tetrafluoro yttrium lithium up-conversion luminescence nanobelt of 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 lithium LiYF that mix of erbium ytterbium 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt, the steps include:
(1) preparation spinning solution
That He Yi source, ,Er source, ,Yi source, lithium source is used is a hydronium(ion) oxidation lithium LiOHH 2o, 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 an a certain amount of hydronium(ion) oxidation lithium LiOHH 2o, yittrium oxide Y 2o 3, erbium oxide Er 2o 3with ytterbium oxide Yb 2o 3, Li 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, obtain LiNO 3, Y (NO 3) 3, Er (NO 3) 3and Yb (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, stir 6h in the room temperature lower magnetic force, and standing 4h, 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/[LiNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band
The spinning solution prepared 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, 20～28 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/[LiNO 3+ Y (NO 3) 3+ Er (NO 3) 3+ Yb (NO 3) 3] the composite Nano band;
(3) prepare the mixed oxide nanoparticle band
By described PVP/[LiNO 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, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature with body of heater afterwards, obtains the mixed oxide nanoparticle band;
(4) prepare LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt
Fluorination reagent is used ammonium acid fluoride NH 4hF 2adopt double crucible method, ammonium acid fluoride is put into to monkey, the above covers carbon-point, described mixed oxide nanoparticle band is placed on above carbon-point, monkey is put into to larger crucible, add excessive ammonium acid fluoride between interior outer crucible, add that on outer crucible the 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 ℃, naturally cool to room temperature with body of heater afterwards, obtain LiYF 4: Er 3+, Yb 3+the up-conversion luminescence nanobelt, width is 7.97 ± 0.32 μ m, and thickness is 69.1nm, and length is greater than 50 μ m.
CN 201210044190 2012-02-24 2012-02-24 Method for preparing erbium and ytterbium double-doped yttrium lithium tetrafluoride up-conversion luminescent nanobelt Expired - Fee Related CN102660801B (en)

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