CN102618969B - Preparation method of europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt - Google Patents

Preparation method of europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt Download PDF

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CN102618969B
CN102618969B CN201210044574.XA CN201210044574A CN102618969B CN 102618969 B CN102618969 B CN 102618969B CN 201210044574 A CN201210044574 A CN 201210044574A CN 102618969 B CN102618969 B CN 102618969B
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nanobelt
pvp
europium
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CN102618969A (en
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董相廷
于飞
王进贤
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 of a europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt and belongs to the technical field of nano material preparation. The preparation method comprises four steps: firstly, preparing a spinning liquor: weighing Na2CO3, Y2O3 and Eu2O3, dissolving the Na2CO3, the Y2O3 and the Eu2O3 with HNO3 and evaporating to obtain a Na2CO3, Y(NO3)3 and Eu2O3 mixed crystal; adding a DMF (Dimethyl Formamide) solvent and a polyvinylpyrrolidone (PVP) to obtain the spinning solution; secondly, preparing a PVP/[NaNO3+Y(NO3)3+Eu(NO3)3] original composite nanobelt by adopting an electrospinning fiber technique; thirdly, preparing a mixed oxide nanobelt: carrying out thermal treatment on the PVP/[NaNO3+Y(NO3)3+Eu(NO3)3] original composite nanobelt to obtain the mixed oxide nanobelt; and fourthly, preparing a NaYE4:5 percent Eu3 red luminescent nanobelt: carrying out fluoridation treatment on the mixed oxide nanobelt to obtain the NaYE4:5 percent Eu3 red luminescent nanobelt by using ammonium hydrogen fluoride through a double-crucible method. The NaYE4:5 percent Eu3 red luminescent nanobelt has excellent crystallization, is 2.21+/-0.27mu m in width, 98.5nm in thickness and more than 50mu in length. The NaYE4:5 percent Eu3 red luminescent nanobelt is a novel red luminescent nano material with important application value. The preparation method disclosed by the invention is simple and feasible, can carry batch production and has a broad application prospect.

Description

A kind of preparation method who mixes europium tetrafluoro yttrium sodium emitting red light nanobelt
Technical field
The present invention relates to nano material preparation research field, relate to specifically a kind of preparation method who mixes europium tetrafluoro yttrium sodium emitting red light nanobelt.
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.
Rare earth tetrafluoride, owing to having abundant 4f energy level and lower phonon energy, is one of current efficient rare-earth ion doping luminous host.Mix europium tetrafluoro yttrium sodium NaYF 4: Eu 3+be a kind of important red illuminating material, there is important application.Adopt the 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 NaYF 4: Eu 3+the nano materials such as nanocrystalline, nanometer rods, sheet, cube is nanocrystalline, hexahedron is nanocrystalline, octahedra nanocrystalline, hollow tubular structures, nano wire, spindle.Mix europium tetrafluoro yttrium sodium NaYF 4: Eu 3+nanobelt is a kind of novel red illuminating 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, have no and mix europium tetrafluoro yttrium sodium NaYF 4: Eu 3+the report of 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: Eu 3+the report of emitting red light 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 3with europium oxide Eu 2o 3for raw material, with evaporating after nitric acid dissolve, obtain sodium nitrate NaNO 3, yttrium nitrate Y (NO 3) 3with europium nitrate Eu (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+ Eu (NO 3) 3] original 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: Eu 3+emitting red light nanobelt.
Summary of the invention
Prior art adopts the 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 NaYF 4: Eu 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 red Illuminant nanometer carrying material is provided in nanobelt field, we combine electrostatic spinning technique with fluorination technology, invented NaYF 4: Eu 3+the preparation method of emitting red light 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+ Eu (NO 3) 3] original 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: Eu 3+emitting red light nanobelt.In the present invention, the mole percent of the europium ion of doping is 5%, is labeled as NaYF 4: 5%Eu 3+, i.e. that the present invention is prepared is NaYF 4: 5%Eu 3+emitting red light nanobelt.The steps include:
(1) preparation spinning solution
That He You source, ,Yi source, sodium source is used is sodium carbonate Na 2cO 3, yittrium oxide Y 2o 3with europium oxide Eu 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 3with europium oxide Eu 2o 3, Na wherein +, Y 3+and Eu 3+mol ratio be 100: 95: 5, the mole percent of europium ion is 5%, uses nitric acid HNO 3after dissolving, evaporation, obtains NaNO 3, Y (NO 3) 3and Eu (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 5h, and standing 3h, 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) prepare PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original 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 16cm, 18～25 ℃ of room temperatures, relative humidity is 50%～75%, obtains PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original composite Nano band;
(3) prepare mixed oxide nanoparticle band
By described PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original 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: 5%Eu 3+emitting red light 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: 5%Eu 3+emitting red light nanobelt, width is 2.21 ± 0.27 μ m, and thickness is 98.5nm, and length is greater than 50 μ m.
At the NaYF described in said process 4: 5%Eu 3+emitting red light nanobelt has good crystallinity, and nanobelt width is 2.21 ± 0.27 μ m, and thickness is 98.5nm, and length is greater than 50 μ m, has realized goal of the invention.
Accompanying drawing explanation
Fig. 1 is NaYF 4: 5%Eu 3+the XRD spectra of emitting red light nanobelt;
Fig. 2 is NaYF 4: 5%Eu 3+the SEM photo of emitting red light nanobelt, this figure doubles as Figure of abstract;
Fig. 3 is NaYF 4: 5%Eu 3+the width distribution histogram of emitting red light nanobelt;
Fig. 4 is NaYF 4: 5%Eu 3+the EDS spectrogram of emitting red light nanobelt;
Fig. 5 is NaYF 4: 5%Eu 3+the exciting light spectrogram of emitting red light nanobelt;
Fig. 6 is NaYF 4: 5%Eu 3+the utilizing emitted light spectrogram of emitting red light nanobelt.
The specific embodiment
The yittrium oxide Y that the present invention is selected 2o 3with europium oxide Eu 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 3with europium oxide Eu 2o 3, Na wherein +, Y 3+and Eu 3+mol ratio be 100: 95: 5, the mole percent of europium ion is 5%, uses nitric acid HNO 3after dissolving, evaporation, obtains NaNO 3, Y (NO 3) 3and Eu (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 5h, and standing 3h, 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 16cm, 18～25 ℃ of room temperatures, relative humidity is 50%～75%, obtains PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original composite Nano band; By described PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original 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: 5%Eu 3+emitting red light nanobelt.Described NaYF 4: 5%Eu 3+emitting red light 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: 5%Eu 3+emitting red light nanobelt is nano strip, and thickness is 98.5nm, and length is greater than 50 μ m, as shown in Figure 2.By Shapiro-Wilk method to NaYF 4: 5%Eu 3+the width of emitting red light nanobelt carries out normal distribution-test, under 95% confidence level, and NaYF 4: 5%Eu 3+the width distribution of emitting red light nanobelt belongs to normal distribution, and width is 2.21 ± 0.27 μ m, as shown in Figure 3.NaYF 4: 5%Eu 3+emitting red light nanobelt forms (the Au conductive layer of plated surface when Au derives from SEM sample preparation) by Na, Y, F and Eu element, as shown in Figure 4.When monitoring wavelength is 592nm, NaYF 4: 5%Eu 3+the strongest excitation peak of emitting red light nanobelt is positioned at 395nm place, corresponding to Eu 3+'s 7f 0→ 5l 6transition, as shown in Figure 5.Under the ultraviolet excitation of 395nm, NaYF 4: 5%Eu 3+emitting red light nanobelt is launched the bright red that main peak is positioned at 592nm and 616nm, 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; 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. a preparation method who mixes europium tetrafluoro yttrium sodium emitting red light nanobelt, 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 europium ion-doped tetrafluoro yttrium sodium NaYF 4: Eu 3+emitting red light nanobelt, the steps include:
(1) preparation spinning solution
That He You source, ,Yi source, sodium source is used is sodium carbonate Na 2cO 3, yittrium oxide Y 2o 3with europium oxide Eu 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 3with europium oxide Eu 2o 3, Na wherein +, Y 3+and Eu 3+mol ratio be 100:95:5, the mole percent of europium ion is 5%, uses nitric acid HNO 3after dissolving, evaporation, obtains NaNO 3, Y (NO 3) 3and Eu (NO 3) 3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 5h, and standing 3h, 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) prepare PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original 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 16cm, 18～25 ℃ of room temperatures, relative humidity is 50%～75%, obtains PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original composite Nano band;
(3) prepare mixed oxide nanoparticle band
By described PVP/[NaNO 3+ Y (NO 3) 3+ Eu (NO 3) 3] original 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: 5%Eu 3+emitting red light 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: 5%Eu 3+emitting red light nanobelt, width is 2.21 ± 0.27 μ m, and thickness is 98.5nm, and length is greater than 50 μ m.
CN201210044574.XA 2012-02-24 2012-02-24 Preparation method of europium-doped sodium tetrafluoro gadolinium red luminescent nanobelt Expired - Fee Related CN102618969B (en)

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CN102817109B (en) * 2012-08-10 2014-07-02 长春理工大学 Preparation method for europium doped yttrium disilicate red luminescence nano-belts
CN106120023B (en) * 2016-07-04 2018-05-22 长春理工大学 A kind of method for preparing er-doped yttrium fluoride barium up-conversion luminescence nanofiber

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CN1876758A (en) * 2006-07-20 2006-12-13 长春理工大学 Low temperature combustion synthesis method for converting luminescent material of fluoride
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

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876758A (en) * 2006-07-20 2006-12-13 长春理工大学 Low temperature combustion synthesis method for converting luminescent material of fluoride
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

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