CN101693832B - Method for preparing rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts - Google Patents
Method for preparing rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts Download PDFInfo
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Abstract
The invention relates to a method for preparing rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts, which belongs to the technical field of nano-material preparation and includes two steps: (1) preparing spinning liquor; (2) preparing the rare-earth complexes/PMMA composite luminescent nanobelts. The first step includes: the rare-earth complexes in the spinning liquor adopt two ligand complexes; the general formula is: RE (BA)3Phen, wherein RE=Eu, Tb, Sm, Nd, BA is benzoic acid, and Phen is phenanthroline; a macromolecule template agent and matrixes adopt polymethyl methacrylate (PMMA); dissolvent employs mixture of chloroform (CHC13) and N, N-dimethylformamide (DMF); weighing a certain amount of the PMMA and dissolving the PMMA in mixed liquor (volume ratio is 15:1) including the chloroform (CHC13) and the DMF; stirring the mixed liquor for 4 hours with a magnetic force in a water bath at 60 DEG C and standing the mixed liquor for 3 hours to obtain even and transparent PMMA liquor with mass percentage concentration of 5%; dissolving a certain amount of the rare-earth complexes in the PMMA liquor, stirring the liquor for 5 hours at room temperature, and then standing the liquor for 2 hours to obtain the PMMA liquor of the rare-earth complexes, namely the spinning liquor; and the mass percentage concentration of the rare-earth complexes ranges from 5% to 20%. The second step includes: adopting electrostatic spinning technology, and using the prepared spinning liquor to prepare the rare-earth complexes/PMMA composite luminescent nanobelts. Further, technical parameters include: a direct current voltage ranges from 6 kilovolts to 10 kilovolts, the inner diameter of a nozzle is 0.6 millimeter, an included angle between the nozzle and a horizontal plane is 30 degrees, solidified distance from the nozzle to a receiving screen ranges from 12 centimeters to 20 centimeters; indoor temperature ranges from18 DEG C to 25 DEG C.
Description
Technical field
The present invention relates to the nano material preparation technical field, relate to a kind of method for preparing the rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts specifically.
Background technology
The preparation of nano belt and property research are one of hot research field, forward position of subject researchs such as Materials science, chemistry, Condensed Matter Physics at present.Nano belt is a kind ofly to be the nano material of zonal structure with the manual method synthetic, and its xsect is a rectangular configuration, and its thickness is in nanometer scale, 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 receive extensive concern.Though nano belt lacks the high structural capacity that the cylindricality nanotube is had, its production process simple controllable, and can guarantee the material structure homogeneous during mass production, do not have defective basically, thereby cause people's great attention.
Rare earth is a huge mine of luminescent materials, and in the various luminescent materials of human development, REE is being brought into play important effect.Because REE has unique electronic structure, performance, the especially REEs such as light, electricity, magnetic that makes rare earth compound show many excellences have general element incomparable spectroscopic properties, so rare earth luminescent material is especially noticeable.Rare earth compounding is widely used in luminous and the demonstration field with its unique fluorescent characteristic, has broad application prospects in fields such as pl-, electroluminescent, laserable material and solar energy converting materials.Though rare earth organic complex has good luminous property, its less stable, thereby limited its application.Rare earth compounding is compound in the organic polymer matrix; The matrix material that is obtained not only has characteristics such as the light, electricity, magnetic of REE; For rare earth ion provides stable chemical environment; Strengthen the rare earth compounding luminescent properties, the while has the macromolecular material light weight again, anti-impact force is strong and the premium properties of easy machine-shaping, makes macromolecular material realize functionalization.China's rare earth resources and output all account for first place, the world, and exploitation rare earth new material, the new and effective rare-earth luminescent material of research have very important realistic meaning.Therefore, rare earth compounding/macromolecule composite luminescent nano belt is not only a kind of nano structural material of novelty, also is the novel rare-earth luminescent material that potential using value is arranged, and its preparation and property research are significant.
The patent No. is the technical scheme that 1975504 USP discloses a relevant electrospinning process (electrospinning); This method is the preparation successive, has a kind of effective ways of the micro nanometer fiber of macro length, 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 macromolecular solution or melt in electrostatic field, to receive the traction of electrostatic force and spray by nozzle; Invest the receiving screen on opposite, thereby realize wire drawing, solvent evaporation at normal temperatures then; Perhaps melt is cooled to normal temperature and solidifies, and obtains micro nanometer fiber.Z.M.Huang et al has reported with method of electrostatic spinning and has prepared multiple polymers nanofiber (Composites Science and Technology; 2003,63,2223-2253); Dong Xiangting etc. have reported that the employing electrostatic spinning technique prepares PVP hollow nano fiber (Changchun University of Science and Technology's journal; 2007,30 (4), 15-18).Existing people utilizes electrostatic spinning technique to prepare high molecular nanometer band (Materials Letters, 2007,61,2325-2328; Journal of Polymer Science:Part B:Polymer Physics, 2001,39,2598-2606), but prepared high molecular nanometer bandwidth is very narrow.Dong Xiangting etc. have reported that the employing electrostatic spinning technique prepares PAN/Eu (BA)
3Phen recombination luminescence nanofiber (New Chemical Materials, 2008,36 (9), 49-52).At present, do not see and utilize electrostatic spinning technique to prepare the relevant report of rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts.Polymethylmethacrylate (PMMA) is a kind of well behaved macromolecular material commonly used.The present invention adopts electrostatic spinning technique, is raw material with the rare earth compounding, and polymethylmethacrylate (PMMA) is as template and matrix; With chloroform and N; Dinethylformamide (DMF) is a solvent, under the processing condition of the best, prepares rare earth compounding/PMMA composite luminescent nanobelts.
Summary of the invention
In background technology, adopt electrostatic spinning technique to prepare PAN/Eu (BA)
3Phen recombination luminescence nanofiber.Use electrostatic spinning technique in the background technology prepares the high molecular nanometer band, and employed raw material, template and processing condition are all different with method of the present invention.The present invention uses electrostatic spinning technique to prepare rare earth compounding/PMMA composite luminescent nanobelts, and bandwidth reaches 10～20 μ m, the about 200nm～500nm of nano belt thickness, and length is greater than 5cm.
The present invention is achieved in that and at first prepares the spinning solution with certain viscosity that is used for electrostatic spinning technique that the viscosity of control spinning solution is most important.Use electrostatic spinning technique and carry out electrostatic spinning, under the processing condition of the best, prepare rare earth compounding/PMMA composite luminescent nanobelts.
The steps include:
(1) preparation spinning solution
Spinning solution middle-weight rare earths title complex adopts two kinds of ligand-complexes, and general formula is: RE (BA)
3Phen, RE=Eu, Tb, Sm, Nd, BA: phenylformic acid, Phen: phenanthroline.High polymer templates and matrix adopt polymethylmethacrylate (PMMA).Solvent adopts chloroform (CHCl
3) and N, the mixture of dinethylformamide (DMF).Take by weighing a certain amount of PMMA, be dissolved in CHCl
3With (volume ratio 15: 1) in the DMF mixed solution, magnetic agitation 4h in 60 ℃ of water-baths leaves standstill 3h afterwards, can obtain homogeneous, transparent, mass percent concentration and be 5% PMMA solution.A certain amount of rare earth compounding is dissolved in the PMMA solution, stirs 5h under the room temperature, leave standstill 2h afterwards, obtain the PMMA solution of rare earth compounding, this is spinning solution, and wherein the mass percent concentration of rare earth compounding is 5%-20%.
(2) preparation rare earth compounding/PMMA composite luminescent nanobelts
Adopt electrostatic spinning technique, use the PMMA solution of above-mentioned rare earth compounding to prepare rare earth compounding/PMMA composite luminescent nanobelts.Technical parameter is: volts DS is 6kV～10kV, and the internal diameter of nozzle is 0.6mm, and the angle of nozzle and horizontal plane is 30 °, and nozzle is 12～20cm to the curing distance of receiving screen; 18～25 ℃ of room temps, relative humidity are 45%～65%.
Rare earth compounding/PMMA composite luminescent nanobelts surface ratio prepared in said process is than smooth, and bandwidth reaches 10～20 μ m, the about 200nm～500nm of nano belt thickness, and length has good luminosity greater than 5cm, has realized goal of the invention.
Description of drawings
Fig. 1 is Eu (BA)
3The SEM photo of Phen/PMMA composite luminescent nanobelts, the double accompanying drawing that makes an abstract of this figure.Fig. 2 is Eu (BA)
3The excitation spectrum of Phen/PMMA composite luminescent nanobelts.Fig. 3 is Eu (BA)
3The emmission spectrum of Phen/PMMA composite luminescent nanobelts.Fig. 4 is Tb (BA)
3The SEM photo of Phen/PMMA composite luminescent nanobelts.Fig. 5 is Tb (BA)
3The excitation spectrum of Phen/PMMA composite luminescent nanobelts.Fig. 6 is Tb (BA)
3The emmission spectrum of Phen/PMMA composite luminescent nanobelts.Fig. 7 is Sm (BA)
3The SEM photo of Phen/PMMA composite luminescent nanobelts.
Embodiment
Embodiment 1: take by weighing a certain amount of PMMA, be dissolved in CHCl
3With (volume ratio 15: 1) in the DMF mixed solution, magnetic agitation 4h in 60 ℃ of water-baths leaves standstill 3h afterwards, can obtain homogeneous, transparent, mass percent concentration and be 5% PMMA solution.With a certain amount of Eu (BA)
3Phen is dissolved in the PMMA solution, stirs 5h under the room temperature, leaves standstill 2h afterwards, obtains Eu (BA)
3The PMMA solution of Phen, this promptly is a spinning solution, wherein Eu (BA)
3The mass percent concentration of Phen is 10%.Carry out electrostatic spinning in the liquid storage pipe with the spinning solution adding device for spinning for preparing, nozzle inside diameter 0.6mm, the angle of adjustment nozzle and horizontal plane is 30 °; Apply the volts DS of 6kV, solidify apart from 12cm 18～25 ℃ of room temperatures; Relative humidity is 45%～65%, obtains Eu (BA)
3The Phen/PMMA composite luminescent nanobelts.Eu (BA)
3Phen/PMMA composite luminescent nanobelts surface ratio is than smooth, and width is even, and bandwidth reaches 15～20 μ m, the about 350nm～500nm of nano belt thickness, and length is seen shown in Figure 1 greater than 6cm.When the monitoring wavelength is 613nm, prepared Eu (BA)
3The excitation spectrum main peak of Phen/PMMA composite luminescent nanobelts is positioned at the strong broad band at 348nm place, sees shown in Figure 2.Under the ultraviolet excitation of 348nm, Eu (BA)
3The Phen/PMMA composite luminescent nanobelts is launched the bright red that main peak is positioned at 613nm, and it is corresponding to Eu
3+Ionic
5D
0→
7F
2Transition belongs to Eu
3+Ionic forces electric dipole transition, sees shown in Figure 3.
Embodiment 2: take by weighing a certain amount of PMMA, be dissolved in CHCl
3With (volume ratio 15: 1) in the DMF mixed solution, magnetic agitation 4h in 60 ℃ of water-baths leaves standstill 3h afterwards, can obtain homogeneous, transparent, mass percent concentration and be 5% PMMA solution.With a certain amount of Tb (BA)
3Phen is dissolved in the PMMA solution, stirs 5h under the room temperature, leaves standstill 2h afterwards, obtains Tb (BA)
3The PMMA solution of Phen, this promptly is a spinning solution, wherein Tb (BA)
3The mass percent concentration of Phen is 10%.Carry out electrostatic spinning in the liquid storage pipe with the spinning solution adding device for spinning for preparing, nozzle inside diameter 0.6mm, the angle of adjustment nozzle and horizontal plane is 30 °; Apply the volts DS of 6kV, solidify apart from 12cm 18～25 ℃ of room temperatures; Relative humidity is 50%～65%, obtains Tb (BA)
3The Phen/PMMA composite luminescent nanobelts.Tb (BA)
3Phen/PMMA composite luminescent nanobelts surface ratio is than smooth, and width is even, and bandwidth reaches 10～20 μ m, the about 200nm～350nm of nano belt thickness, and length is seen shown in Figure 4 greater than 5cm.When the monitoring wavelength is 543nm, prepared Tb (BA)
3The excitation spectrum main peak of Phen/PMMA composite luminescent nanobelts is positioned at the strong broad band at 298nm place, sees shown in Figure 5.Under the ultraviolet excitation of 298nm, Tb (BA)
3The Phen/PMMA composite luminescent nanobelts is launched the bright green glow that main peak is positioned at 543nm, and it is corresponding to Tb
3+Ionic
5D
4→
7F
5Transition is seen shown in Figure 6.
Embodiment 3: take by weighing a certain amount of PMMA, be dissolved in CHCl
3With (volume ratio 15: 1) in the DMF mixed solution, magnetic agitation 4h in 60 ℃ of water-baths leaves standstill 3h afterwards, can obtain homogeneous, transparent, mass percent concentration and be 5% PMMA solution.With a certain amount of Sm (BA)
3Phen is dissolved in the PMMA solution, stirs 5h under the room temperature, leaves standstill 2h afterwards, obtains Sm (BA)
3The PMMA solution of Phen, this promptly is a spinning solution, wherein Sm (BA)
3The mass percent concentration of Phen is 5%.Carry out electrostatic spinning in the liquid storage pipe with the spinning solution adding device for spinning for preparing, nozzle inside diameter 0.6mm, the angle of adjustment nozzle and horizontal plane is 30 °; Apply the volts DS of 10kV, solidify apart from 20cm 18～25 ℃ of room temperatures; Relative humidity is 45%～65%, obtains Sm (BA)
3The Phen/PMMA composite luminescent nanobelts.This nano belt surface ratio is than smooth, and width is even, and bandwidth reaches 15～20 μ m, the about 300nm～450nm of nano belt thickness, and length is seen shown in Figure 7 greater than 5cm.
Embodiment 4: take by weighing a certain amount of PMMA, be dissolved in CHCl
3With (volume ratio 15: 1) in the DMF mixed solution, magnetic agitation 4h in 60 ℃ of water-baths leaves standstill 3h afterwards, can obtain homogeneous, transparent, mass percent concentration and be 5% PMMA solution.With a certain amount of Nd (BA)
3Phen is dissolved in the PMMA solution, stirs 5h under the room temperature, leaves standstill 2h afterwards, obtains Nd (BA)
3The PMMA solution of Phen, this promptly is a spinning solution, wherein Nd (BA)
3The mass percent concentration of Phen is 20%.Carry out electrostatic spinning in the liquid storage pipe with the spinning solution adding device for spinning for preparing, nozzle inside diameter 0.6mm, the angle of adjustment nozzle and horizontal plane is 30 °; Apply the volts DS of 8kV, solidify apart from 16cm 18～25 ℃ of room temperatures; Relative humidity is 45%～65%, obtains Nd (BA)
3The Phen/PMMA composite luminescent nanobelts.This nano belt bandwidth reaches 15～20 μ m, the about 400nm～500nm of nano belt thickness, and length is greater than 6cm.
The phenylformic acid that the present invention selected for use, phenanthroline, chloroform, DMF, nitric acid are commercially available analytical pure product, and the purity of rare earth oxide is 99.99%.Utilize rare earth oxide, nitric acid, phenylformic acid, phenanthroline self-control rare earth compounding.PMMA is homemade, and molecular-weight average is about 100000.Used glassware and equipment are commonly used in the laboratory.
Claims (4)
1. method for preparing the rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts; It is characterized in that; Use electrostatic spinning technique, use polymethylmethacrylate (PMMA) to be high polymer templates and matrix, adopting the mixture of the different solvent of two kinds of evaporation rates is solvent; The preparation product is the rare-earth complexes/polymethyl methacrylate composite luminescent nanobelts, the steps include:
(1) preparation spinning solution
Spinning solution middle-weight rare earths title complex adopts two kinds of ligand-complexes, and general formula is: RE (BA)
3Phen, RE=Eu, Tb, Sm, Nd, BA: phenylformic acid, Phen: phenanthroline, high polymer templates and matrix adopt polymethylmethacrylate (PMMA), and solvent adopts chloroform (CHCl
3) and N, the mixture of dinethylformamide (DMF) takes by weighing a certain amount of PMMA, is dissolved in CHCl
3In the DMF mixed solution, magnetic agitation 4h in 60 ℃ of water-baths leaves standstill 3h afterwards; Can obtain homogeneous, transparent, mass percent concentration and be 5% PMMA solution, a certain amount of rare earth compounding is dissolved in the PMMA solution, stir 5h under the room temperature; Leave standstill 2h afterwards, obtain the PMMA solution of rare earth compounding, this is spinning solution; Wherein the mass percent concentration of rare earth compounding is 5%-20%, described CHCl
3With the DMF mixed solution, it is characterized in that CHCl
3With the volume ratio of DMF be 15: 1;
(2) preparation rare earth compounding/PMMA composite luminescent nanobelts
Adopt electrostatic spinning technique; Use the spinning solution of above-mentioned preparation to prepare rare earth compounding/PMMA composite luminescent nanobelts; Technical parameter is: volts DS is 6kV～10kV; The internal diameter of nozzle is 0.6mm, and the angle of nozzle and horizontal plane is 30 °, and nozzle is 12～20cm to the curing distance of receiving screen; 18～25 ℃ of room temps, relative humidity are 45%～65%.
2. the preparation method of rare earth compounding according to claim 1/PMMA composite luminescent nanobelts is characterized in that, the mass percent concentration of spinning solution middle-weight rare earths title complex is in 5%, 10% and 20%.
3. the preparation method of rare earth compounding according to claim 1/PMMA composite luminescent nanobelts is characterized in that, electrostatic spinning voltage is among 6kV, 8kV and the 10kV.
4. the preparation method of rare earth compounding according to claim 1/PMMA composite luminescent nanobelts is characterized in that, nozzle is among 12cm, 16cm and the 20cm to the curing distance of receiving screen.
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| US4058965A (en) * | 1974-07-03 | 1977-11-22 | Platt Saco Lowell Limited | Open-end spinning machines |
| CN101235558A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber |
| CN101348951A (en) * | 2008-07-11 | 2009-01-21 | 长春理工大学 | Preparation of rare earth fluoride/rare earth oxyfluoride composite nano fibre |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4058965A (en) * | 1974-07-03 | 1977-11-22 | Platt Saco Lowell Limited | Open-end spinning machines |
| CN101235558A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber |
| CN101348951A (en) * | 2008-07-11 | 2009-01-21 | 长春理工大学 | Preparation of rare earth fluoride/rare earth oxyfluoride composite nano fibre |
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