CN102817094A - Method for preparing europium doped yttrium disilicate red luminescence nano-fibers - Google Patents

Method for preparing europium doped yttrium disilicate red luminescence nano-fibers Download PDF

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CN102817094A
CN102817094A CN201210288301XA CN201210288301A CN102817094A CN 102817094 A CN102817094 A CN 102817094A CN 201210288301X A CN201210288301X A CN 201210288301XA CN 201210288301 A CN201210288301 A CN 201210288301A CN 102817094 A CN102817094 A CN 102817094A
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europium
pvp
nano
nanofiber
fibers
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王进贤
董相廷
张誉腾
毕菲
于文生
刘桂霞
浦利
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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 present invention relates to a method for preparing europium-doped yttrium disilicate red luminescence nano-fibers, and belongs to the technical field of nano-material preparation. In the prior art, Y2Si2O7:5%Eu<3+> micrometer particles or nano-particles are prepared. The preparation method of the present invention comprises the following three steps: (1) preparing a spinning solution; (2) adopting an electrostatic spinning technology to prepare PVP/[Y(NO3)3+Eu(NO3)3+Si(C2H5O)4] composite fibers; (3) preparing Y2Si2O7:5%Eu<3+> nano-fibers, wherein the composite fibers are subjected to a heat treatment in air to obtain the Y2Si2O7:5%Eu<3+> nano-fibers, and the Y2Si2O7:5%Eu<3+> nano-fibers have characteristics of good crystallinity, an average diameter of 180 nm, and a length more than 100 mum, and are a novel red nanometer luminescence material. The preparation method of the present invention has characteristics of simpleness, easy performing, mass production, and broad application prospects.

Description

The method of europium disilicic acid red yttrium luminous nano fibre is mixed in a kind of preparation
Technical field
The present invention relates to the nano material preparation technical field, relate to the method that europium disilicic acid red yttrium luminous nano fibre is mixed in a kind of preparation specifically.
Background technology
Nanofiber is meant the filamentary material that on the three dimensions yardstick of material, has bidimensional to be in nanoscale, and radial dimension is a nanometer scale usually, and length is then bigger.Because the radial dimension of nanofiber is little of nanometer scale; Demonstrate series of characteristics; The most outstanding is that specific area is big; Thereby its surface energy increases with active, and then produces small-size effect, surface or interfacial effect, quantum size effect, macro quanta tunnel effect etc., and therefore shows the specificity of a series of chemistry, physics (heat, light, sound, electricity, magnetic etc.) aspect.In the prior art, a lot of methods that prepare nanofiber are arranged, the method for for example reeling off raw silk from cocoons, template synthetic method, split-phase method and self-assembly method etc.In addition, also has arc evaporation, laser high temperature inustion, compound pyrolysismethod.These three kinds of methods in fact all are after at high temperature making compound (or simple substance) evaporation, make nanofiber or nanotube through pyrolysis (or directly condensation), from essence, all belong to the compound steam sedimentation.
Disilicic acid yttrium Y 2Si 2O 7Have low elastic modulus, lower thermal conductivity, low vaporization at high temperature rate, low high-temperature oxygen permeability, low linear expansion coefficient, resistance to chemical attack and higher chemistry and thermodynamic stability, make Y 2Si 2O 7Material has broad application prospects, as is applied to high-temperature structural ceramics, the matrix of rare earth luminescence material etc.Y 2Si 2O 7Multiple crystalline phase is arranged, and along with the variation of synthesis temperature, these crystalline phases can transform each other, and are accompanied by very big Volume Changes during these crystal transitions, therefore synthetic single-phase Y 2Si 2O 7Very difficult.Mix europium disilicic acid yttrium Y 2Si 2O 7: Eu 3+It is a kind of important red fluorescence material.At present, Y 2Si 2O 7: Eu 3+The main methods such as high temperature solid-state method, sol-gel process, firing method, hydro-thermal method, presoma pyrolysismethod that adopt are synthesized, and synthetic product is Y 2Si 2O 7: Eu 3+Micron particles or nano particle.Mix europium disilicic acid yttrium Y 2Si 2O 7: Eu 3+Nanofiber 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 at present the Y of pure phase 2Si 2O 7: Eu 3+The report of nanofiber.
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.Employing electrostatic spinning techniques such as Dong Xiangting have prepared mixes europium Y 7O 6F 9Nanofiber [Chinese invention patent, grant number: ZL201010550196.3]; Employing electrostatic spinning techniques such as Wang Jinxian have prepared rare earth trifluoride nanofiber [Chinese invention patent, grant number: ZL201010107993.4].Electrospinning process can prepare big L/D ratio micrometer fibers or nanofiber continuously.At present, do not see that the employing electrostatic spinning technique prepares Y 2Si 2O 7: Eu 3+The report of emitting red light nanofiber.
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 ethyl orthosilicate Si (C 2H 5O) 4, adding solvent N again, 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+ Si (C 2H 5O) 4] composite fibre, it is heat-treated in air, obtain the Y of the pure phase of novel structure 2Si 2O 7: Eu 3+Nanofiber.
Summary of the invention
Various in background technology prepare in the method for nanofiber, the shortcoming of the method for reeling off raw silk from cocoons be solution viscosity is required too harsh; The shortcoming of template synthetic method is to prepare the continuous fibers that the root root separates; Split-phase method and self-assembly method production efficiency are all lower; And the compound steam sedimentation is because to the demand of high temperature, so process conditions are difficult to control, and the nanofiber major diameter of above-mentioned several method preparation is than little.Use electrostatic spinning technique in the background technology has prepared metal oxide, composite oxide of metal nanofiber, europium Y 7O 6F 9, rare earth trifluoride nanofiber.Prior art adopts methods such as high temperature solid-state method, sol-gel process, firing method, hydro-thermal method, presoma pyrolysismethod to synthesize Y 2Si 2O 7: Eu 3+Micron particles or nano particle.For a kind of novel red luminous nano fibre material is provided in the nanofiber field, we have invented a kind of preparation Y 2Si 2O 7: Eu 3+The method of emitting red light nanofiber.
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+ Si (C 2H 5O) 4] composite fibre, it is heat-treated in air, obtained the Y of the pure phase of novel structure 2Si 2O 7: Eu 3+Nanofiber.In the present invention, the mole percent of the europium ion of doping is 5%, is labeled as Y 2Si 2O 7: 5%Eu 3+, i.e. that the present invention is prepared is Y 2Si 2O 7: 5%Eu 3+The emitting red light nanofiber.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 1300000, 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 ethyl orthosilicate Si (C 2H 5O) 4, make Y 3++ Eu 3+With Si (C 2H 5O) 4Mol ratio be 1: 1, add an amount of N again, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 4h in the room temperature lower magnetic force; And leave standstill 2h, and forming spinning solution, the mass percent of this each part of spinning solution is: salt content 8%; PVP content 12%, solvent DMF content 80%;
(2) preparation PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre
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 angle of adjustment shower nozzle and horizontal plane is 15 °, applies the DC voltage of 14kV, solidifies apart from 20cm; 15～25 ℃ of room temperatures, relative humidity is 50%～70%, obtains PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre;
(3) preparation Y 2Si 2O 7: 5%Eu 3+Nanofiber
With described PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 1000 ℃ of constant temperature 8h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 2Si 2O 7: 5%Eu 3+Nanofiber, average diameter are 180nm, and length is greater than 100 μ m.
At the Y described in the said process 2Si 2O 7: 5%Eu 3+Nanofiber has good crystallinity, and average diameter is 180nm, and length has realized goal of the invention greater than 100 μ m.
Description of drawings
Fig. 1 is Y 2Si 2O 7: 5%Eu 3+The XRD spectra of nanofiber;
Fig. 2 is Y 2Si 2O 7: 5%Eu 3+The SEM photo of nanofiber, this figure double as Figure of abstract;
Fig. 3 is Y 2Si 2O 7: 5%Eu 3+The EDS spectrogram of nanofiber;
Fig. 4 is Y 2Si 2O 7: 5%Eu 3+The exciting light spectrogram of nanofiber;
Fig. 5 is Y 2Si 2O 7: 5%Eu 3+The emission spectrum figure of nanofiber.
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 1300000, N, dinethylformamide DMF, ethyl orthosilicate Si (C 2H 5O) 4With 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 ethyl orthosilicate Si (C 2H 5O) 4, make Y 3++ Eu 3+With Si (C 2H 5O) 4Mol ratio be 1: 1, add an amount of N again, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 4h in the room temperature lower magnetic force; And leave standstill 2h, and forming spinning solution, the mass percent of this each part of spinning solution is: salt content 8%; PVP content 12%, solvent DMF content 80%; 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 angle of adjustment shower nozzle and horizontal plane is 15 °, applies the DC voltage of 14kV, solidifies apart from 20cm; 15～25 ℃ of room temperatures, relative humidity is 50%～70%, obtains PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre; With described PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 1000 ℃ of constant temperature 8h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 2Si 2O 7: 5%Eu 3+Nanofiber.Described Y 2Si 2O 7: 5%Eu 3+Nanofiber has good crystallinity, the d value of its diffraction maximum and relative intensity and Y 2Si 2O 7The listed d value of PDF standard card (74-1994) consistent with relative intensity, belong to monoclinic system, space group is P2 1/ m sees shown in Figure 1.Described Y 2Si 2O 7: 5%Eu 3+The diameter of nanofiber is even, is fibrous, and average diameter is 180nm, and length is seen shown in Figure 2 greater than 100 μ m.Y 2Si 2O 7: 5%Eu 3+Nanofiber is made up of Y, Si, O and Eu element, and the Au conductive layer of surface plating was seen shown in Figure 3 when Au derived from the SEM sample preparation.When the monitoring wavelength is 588nm, Y 2Si 2O 7: 5%Eu 3+The excitation spectrum highest peak of nanofiber is positioned at the 225nm place, belongs to O 2--Eu 3+Between electric charge migration band, see shown in Figure 4.Under the ultraviolet excitation of 225nm, Y 2Si 2O 7: 5%Eu 3+Nanofiber is launched the bright red that main peak is positioned at 588nm, and it is corresponding to Eu 3+Ion 5D 0→ 7F 1Transition is seen 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. one kind prepares the method for mixing europium disilicic acid red yttrium luminous nano fibre, it is characterized in that, adopts electrostatic spinning technique; Use polyvinylpyrrolidone PVP to be high polymer templates; Adopt N, dinethylformamide DMF is a solvent, and the preparation product is for mixing europium disilicic acid yttrium Y 2Si 2O 7: 5%Eu 3+Nanofiber 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, 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 ethyl orthosilicate Si (C 2H 5O) 4, make Y 3++ Eu 3+With Si (C 2H 5O) 4Mol ratio be 1: 1, add an amount of N again, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP; Stir 4h in the room temperature lower magnetic force; And leave standstill 2h, and forming spinning solution, the mass percent of this each part of spinning solution is: salt content 8%; PVP content 12%, solvent DMF content 80%;
(2) preparation PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre
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 angle of adjustment shower nozzle and horizontal plane is 15 °, applies the DC voltage of 14kV, solidifies apart from 20cm; 15～25 ℃ of room temperatures, relative humidity is 50%～70%, obtains PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre;
(3) preparation Y 2Si 2O 7: 5%Eu 3+Nanofiber
With described PVP/ [Y (NO 3) 3+ Eu (NO 3) 3+ Si (C 2H 5O) 4] composite fibre is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 1000 ℃ of constant temperature 8h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 2Si 2O 7: 5%Eu 3+Nanofiber, average diameter are 180nm, and length is greater than 100 μ m.
2. the method for europium disilicic acid red yttrium luminous nano fibre is mixed in a kind of preparation according to claim 1, it is characterized in that, high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=1300000.
CN201210288301XA 2012-08-10 2012-08-10 Method for preparing europium doped yttrium disilicate red luminescence nano-fibers Pending CN102817094A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105780104A (en) * 2016-01-29 2016-07-20 陕西科技大学 Yb2Si2O7 crystal whiskers and preparation method thereof
CN105780120A (en) * 2016-01-29 2016-07-20 陕西科技大学 Y2Si2O7 crystal whiskers and preparation method thereof
CN108977936A (en) * 2018-06-08 2018-12-11 长春理工大学 Coated with silica mixes the preparation method of europium gadolinium fluoride pipe sleeve linear nano fiber
CN110670171A (en) * 2019-10-14 2020-01-10 齐齐哈尔大学 Preparation method of compact yttrium silicate ceramic fiber

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102605473A (en) * 2012-02-24 2012-07-25 长春理工大学 Preparation method of nickel sulfide nanobelts
CN102605469A (en) * 2012-02-24 2012-07-25 长春理工大学 Method for preparing Eu (europium)-doped Y4Al2O9 red luminescent nano fiber
CN102602898A (en) * 2012-02-24 2012-07-25 长春理工大学 Method for preparing monodisperse zinc selenide particles

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102605473A (en) * 2012-02-24 2012-07-25 长春理工大学 Preparation method of nickel sulfide nanobelts
CN102605469A (en) * 2012-02-24 2012-07-25 长春理工大学 Method for preparing Eu (europium)-doped Y4Al2O9 red luminescent nano fiber
CN102602898A (en) * 2012-02-24 2012-07-25 长春理工大学 Method for preparing monodisperse zinc selenide particles

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105780104A (en) * 2016-01-29 2016-07-20 陕西科技大学 Yb2Si2O7 crystal whiskers and preparation method thereof
CN105780120A (en) * 2016-01-29 2016-07-20 陕西科技大学 Y2Si2O7 crystal whiskers and preparation method thereof
CN108977936A (en) * 2018-06-08 2018-12-11 长春理工大学 Coated with silica mixes the preparation method of europium gadolinium fluoride pipe sleeve linear nano fiber
CN108977936B (en) * 2018-06-08 2020-10-13 长春理工大学 Preparation method of silica-coated europium-doped gadolinium fluoride pipe sleeved linear nanofiber
CN110670171A (en) * 2019-10-14 2020-01-10 齐齐哈尔大学 Preparation method of compact yttrium silicate ceramic fiber
CN110670171B (en) * 2019-10-14 2022-03-29 齐齐哈尔大学 Preparation method of compact yttrium silicate ceramic fiber

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Application publication date: 20121212