CN102605470A - Preparation method of europium-doped Y4Al2O9 red light-emitting nanobelt - Google Patents

Preparation method of europium-doped Y4Al2O9 red light-emitting nanobelt Download PDF

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CN102605470A
CN102605470A CN2012100429643A CN201210042964A CN102605470A CN 102605470 A CN102605470 A CN 102605470A CN 2012100429643 A CN2012100429643 A CN 2012100429643A CN 201210042964 A CN201210042964 A CN 201210042964A CN 102605470 A CN102605470 A CN 102605470A
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preparation
nanobelt
pvp
y4al2o9
europium
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董相廷
秦菲
王进贤
于文生
刘桂霞
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Changchun University of Science and Technology
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Changchun University of Science and Technology
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Abstract

The invention relates to a preparation method of an europium-doped Y4Al2O9 red light-emitting nanobelt, belonging to the technical field of nanometer material preparation. Y4Al2O9:Eu<3+> micro-particles or nano-particles are prepared in the prior art. According to the preparation method disclosed by the invention, an Y4Al2O9:5%Eu<3+> nanobelt is prepared by adopting an electro-spinning technology. The preparation method comprises the three steps of: (1) preparation of a spinning solution, to be specific, weighing Y2O3 and Eu2O3, dissolving the Y2O3 and the Eu2O3 by using diluted HNO3 and then vaporizing to obtain Y(NO3)3 and Eu(NO3)3 mixed crystals, adding Al(NO3)3.9H2O, a DMF solvent and PVP (Polyvinylpyrrolidone) to obtain the spinning solution; (2) preparing an original PVP/[Y(NO3)+Eu(NO3)3+Al(NO3)3] composite nanobelt by adopting an electro-spinning technique; and (3) preparation of a Y4Al2O9:5%Eu<3+> nanobelt, to be specific, performing a heat treatment on the original PVP/[Y(NO3)+Eu(NO3)3+Al(NO3)3] composite nanobelt to obtain the Y4Al2O9:5%Eu<3+> nanobelt which is good in crystallinity, 0.4-1.1 mum in width, 89 nm in thickness and more than 50 mum in length. The Y4Al2O9:Eu<3+> nanobelt is an important novel red nanometer light-emitting material and can play an important role in the fields, such as light emission and display, anti-counterfeiting, biological markers and nanometer devices. The preparation method disclosed by the invention has the advantages of being simple and practical, being capable of producing in batches and having wide application prospect.

Description

A kind of europium Y that mixes 4Al 2O 9The preparation method of emitting red light nano belt
Technical field
The present invention relates to the nano material preparation technical field, relate to a kind of europium Y that mixes specifically 4Al 2O 9The preparation method of emitting red light nano belt.
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.
Mix europium yttrium aluminate Y 4Al 2O 9: Eu 3+It is a kind of important red fluorescence material.At present, Y 4Al 2O 9: Eu 3+Material mainly adopts methods such as high temperature solid-state method, sol-gel process, microwave method, firing method, laser ablation method, presoma pyrolysismethod to synthesize, and synthetic product is Y 4Al 2O 9: Eu 3+Micron particles or nano particle.Mixing europium yttrium aluminate nano belt is a kind of important novel red nano luminescent material, will obtain important application in fields such as luminous and demonstration, false proof, biomarker, nano-devices, has broad application prospects.Do not see Y at present 4Al 2O 9: Eu 3+The report of nano belt.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning); This method is a kind of effective ways that prepare continuous, as to have macro length micro nanometer fiber, is at first proposed in 1934 by Formhals.This method mainly is used for preparing high polymer nanometer fiber; It is characterized in that making charged Polymer Solution or melt in electrostatic field, to receive the traction of electrostatic force and spray, invest the receiving screen on opposite, thereby realize wire drawing by nozzle; Then; Solvent evaporation at normal temperatures, perhaps melt is cooled to normal temperature and solidifies, and obtains micro nanometer fiber.Over nearly 10 years, occurred adopting electrospinning process to prepare the technical scheme of inorganic compound such as oxidate nano fiber at the inorfil preparing technical field, described oxide comprises TiO 2, ZrO 2, Y 2O 3, Y 2O 3: RE 3+(RE 3+=Eu 3+, Tb 3+, Er 3+, Yb 3+/ Er 3+), NiO, Co 3O 4, Mn 2O 3, Mn 3O 4, CuO, SiO 2, Al 2O 3, V 2O 5, ZnO, Nb 2O 5, MoO 3, CeO 2, LaMO 3(M=Fe, Cr, Mn, Co, Ni, Al), Y 3Al 5O 12, La 2Zr 2O 7Deng metal oxide and composite oxide of metal.Existing people utilizes electrostatic spinning technique successfully to prepare high molecular nanometer band (Materials Letters, 2007,61:2325-2328; Journal of Polymer Science: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).Employing electrostatic spinning techniques such as Dong Xiangting prepared rare earth fluoride nanobelt (Chinese invention patent, application number: 201010108039.7), titanium dioxide nano-belts (Chinese invention patent, ZL200810050948.2) and Gd 3Ga 5O 12: Eu 3+Porous nano-belt (SCI, 2010,31 (7), 1291-1296).Do not see at present and adopt electrostatic spinning technique to prepare Y 4Al 2O 9: Eu 3+The report of 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 yittrium oxide Y 2O 3With europium oxide Eu 2O 3Be raw material,, obtain Y (NO with evaporating behind the dilute nitric acid dissolution 3) 3And Eu (NO 3) 3Mixed crystal adds ANN aluminium nitrate nonahydrate Al (NO 3) 39H 2O adds solvent N again, 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/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band, it is heat-treated in air, obtain the Y of the pure phase of novel structure 4Al 2O 9: Eu 3+Nano belt.
Summary of the invention
Prior art adopts methods such as high temperature solid-state method, sol-gel process, microwave method, firing method, laser ablation method, presoma pyrolysismethod to synthesize Y 4Al 2O 9: Eu 3+Micron particles or nano particle.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 fluoride nanobelt.For a kind of novel red Illuminant nanometer carrying material is provided in the nano belt field, we have invented a kind of preparation Y 4Al 2O 9: Eu 3+The method of 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/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band, it is heat-treated in air, obtained the Y of the pure phase of novel structure 4Al 2O 9: Eu 3+Nano belt.In the present invention, the mole percent of the europium ion of doping is 5%, is labeled as Y 4Al 2O 9: 5%Eu 3+, i.e. that the present invention is prepared is Y 4Al 2O 9: 5%Eu 3+Nano belt.The steps include:
(1) preparing spinning solution
That use in yttrium source and europium source is yittrium oxide Y 2O 3With europium oxide Eu 2O 3, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 90000, adopts N, and dinethylformamide DMF is a solvent, takes by weighing a certain amount of yittrium oxide Y 2O 3With europium oxide Eu 2O 3, both mol ratios are 95: 5, promptly the mole percent of europium ion is 5%, with rare nitric acid HNO 3The evaporation of dissolving back obtains Y (NO 3) 3And Eu (NO 3) 3Mixed crystal adds ANN aluminium nitrate nonahydrate Al (NO 3) 39H 2O makes Y 3++ Eu 3+With Al 3+Mol ratio be 2: 1, add an amount of N again, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 6h in the room temperature lower magnetic force; And leave standstill 3h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 10%; PVP content 23%, solvent DMF content 67%;
(2) preparation PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original 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 10kV, solidifies apart from 10cm; 18～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band;
(3) preparation Y 4Al 2O 9: 5%Eu 3+Nano belt
With described PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band is put in the temperature programmed control stove and heat-treats, heating rate is 2 ℃/min, at 1100 ℃ of constant temperature 3h, the speed with 2 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 4Al 2O 9: 5%Eu 3+Nano belt, width are 0.4～1.1 μ m, and thickness is 89nm, and length is greater than 50 μ m.
At the Y described in the said process 4Al 2O 9: 5%Eu 3+Nano belt has good crystallinity, and width is 0.4～1.1 μ m, and thickness is 89nm, and length has realized goal of the invention greater than 50 μ m.
Description of drawings
Fig. 1 is Y 4Al 2O 9: 5%Eu 3+The XRD spectra of nano belt;
Fig. 2 is Y 4Al 2O 9: 5%Eu 3+The SEM photo of nano belt, this figure double as Figure of abstract;
Fig. 3 is Y 4Al 2O 9: 5%Eu 3+The EDS spectrogram of nano belt;
Fig. 4 is Y 4Al 2O 9: 5%Eu 3+The exciting light spectrogram of nano belt;
Fig. 5 is Y 4Al 2O 9: 5%Eu 3+The emission spectrum figure of nano belt.
The specific embodiment
The yittrium oxide Y that the present invention selected for use 2O 3With europium oxide Eu 2O 3Purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 90000, N, dinethylformamide DMF, ANN aluminium nitrate nonahydrate Al (NO 3) 39H 2O and 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 yittrium oxide Y 2O 3With europium oxide Eu 2O 3, both mol ratios are 95: 5, promptly the mole percent of europium ion is 5%, with rare nitric acid HNO 3The evaporation of dissolving back obtains Y (NO 3) 3And Eu (NO 3) 3Mixed crystal adds ANN aluminium nitrate nonahydrate Al (NO 3) 39H 2O makes Y 3++ Eu 3+With Al 3+Mol ratio be 2: 1, add an amount of N again, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 6h in the room temperature lower magnetic force; And leave standstill 3h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 10%; PVP content 23%, solvent DMF content 67%; 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 10kV, solidifies apart from 10cm; 18～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band; With described PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band is put in the temperature programmed control stove and heat-treats, heating rate is 2 ℃/min, at 1100 ℃ of constant temperature 3h, the speed with 2 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 4Al 2O 9: 5%Eu 3+Nano belt.Described Y 4Al 2O 9: 5%Eu 3+Nano belt has good crystallinity, the d value of its diffraction maximum and relative intensity and Y 4Al 2O 9The listed d value of PDF standard card (34-0368) consistent with relative intensity, belong to monoclinic system, space group is P21/a, sees shown in Figure 1.Described Y 4Al 2O 9: 5%Eu 3+The width of nano belt is 0.4～1.1 μ m, and thickness is 89nm, and length is seen shown in Figure 2 greater than 50 μ m.Y 4Al 2O 9: 5%Eu 3+Nano belt is formed (the Au conductive layer of surface plating when Au derives from the SEM sample preparation) by Y, Al, O and Eu element, sees shown in Figure 3.When the monitoring wavelength is 609nm, Y 4Al 2O 9: 5%Eu 3+The excitation spectrum highest peak of nano belt is positioned at the 250nm place, belongs to O 2--Eu 3+Between electric charge migration band, see shown in Figure 4.Under the ultraviolet excitation of 250nm, Y 4Al 2O 9: 5%Eu 3+Nano belt is launched the bright red that main peak is positioned at 609nm, and it is corresponding to Eu 3+Ion 5D 0→ 7F 2Transition belongs to Eu 3+Force electric dipole transition, see shown in Figure 5.
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. mix europium Y for one kind 4Al 2O 9The preparation method of emitting red light nano belt is characterized in that, adopts electrostatic spinning technique, uses polyvinylpyrrolidone PVP to be high polymer templates, adopts N, and dinethylformamide DMF is a solvent, and the preparation product is europium ion-doped yttrium aluminate Y 4Al 2O 9: 5%Eu 3+Nano belt the steps include:
(1) preparing spinning solution
Take by weighing a certain amount of yittrium oxide Y 2O 3With europium oxide Eu 2O 3, both mol ratios are 95: 5, promptly the mole percent of europium ion is 5%, with rare nitric acid HNO 3The evaporation of dissolving back obtains Y (NO 3) 3And Eu (NO 3) 3Mixed crystal adds ANN aluminium nitrate nonahydrate Al (NO 3) 39H 2O makes Y 3++ Eu 3+With Al 3+Mol ratio be 2: 1, add an amount of N again, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 6h in the room temperature lower magnetic force; And leave standstill 3h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 10%; PVP content 23%, solvent DMF content 67%;
(2) preparation PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original 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 10kV, solidifies apart from 10cm; 18～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band;
(3) preparation Y 4Al 2O 9: 5%Eu 3+Nano belt
With described PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Al (NO 3) 3] original composite Nano band is put in the temperature programmed control stove and heat-treats, heating rate is 2 ℃/min, at 1100 ℃ of constant temperature 3h, the speed with 2 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 4Al 2O 9: 5%Eu 3+Nano belt, width are 0.4～1.1 μ m, and thickness is 89nm, and length is greater than 50 μ m.
2. a kind of europium Y that mixes according to claim 1 4Al 2O 9The preparation method of emitting red light nano belt is characterized in that, high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=90000.
CN2012100429643A 2012-02-24 2012-02-24 Preparation method of europium-doped Y4Al2O9 red light-emitting nanobelt Pending CN102605470A (en)

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Cited By (2)

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CN102817109A (en) * 2012-08-10 2012-12-12 长春理工大学 Preparation method for europium doped yttrium disilicate red luminescence nano-belts
CN109759050A (en) * 2017-11-09 2019-05-17 吉林建筑大学 Titanium dioxide/terbium ion doping yttrium-aluminium-garnet composite Nano band and its preparation process

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CN101235557A (en) * 2008-03-12 2008-08-06 长春理工大学 Method for preparing rare earth garnet type compound nano fiber
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102817109A (en) * 2012-08-10 2012-12-12 长春理工大学 Preparation method for europium doped yttrium disilicate red luminescence nano-belts
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
CN109759050A (en) * 2017-11-09 2019-05-17 吉林建筑大学 Titanium dioxide/terbium ion doping yttrium-aluminium-garnet composite Nano band and its preparation process
CN109759050B (en) * 2017-11-09 2021-11-16 吉林建筑大学 Titanium dioxide/terbium ion doped yttrium aluminum garnet composite nanobelt and preparation process thereof

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Application publication date: 20120725