CN103397402A - Preparation method of ionic liquid-doped conductive nanofiber - Google Patents
Preparation method of ionic liquid-doped conductive nanofiber Download PDFInfo
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Abstract
The invention belongs to the field of nanofiber preparation technology, and relates to a preparation method of ionic liquid-doped conductive nanofiber. The preparation method comprises the steps of: firstly, preparing ionic liquid 1-ethyl-3-methylimidazolium acetate doped poly(3,4-ethylenedioxythiophene)/sodium polystyrene sulfonate precursor spinning solution, then preparing order ionic solution doped poly(3,4-ethylenedioxythiophene)/sodium polystyrene sulfonate nanofiber and then winding into a poly(3,4-ethylenedioxythiophene)/sodium polystyrene sulfonate nanofiber stranded conductor, and then conducting conductivity property testing on the prepared poly(3,4-ethylenedioxythiophene)/sodium polystyrene sulfonate nanofiber stranded conductor. The method is simple, convenient to operate and repeat, low in cost and strong in practicability, and the prepared ionic liquid-doped conductive nanofiber is good in conductivity property and tensile property and wide to apply.
Description
Technical field:
The invention belongs to the nanofiber preparing technical field, relate to a kind of technique, particularly a kind of preparation method of the ionic liquid conductive-nano-fibers of adulterating that adopts electrostatic spinning technique to prepare poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nanofiber of ionic liquid doping.
Background technology:
conducting polymer, polyacetylene for example, polyaniline, polypyrrole and polythiophene are due to its application prospect widely, caused showing great attention to of people, poly-ethylenedioxy thiophene (PEDOT) is a kind of novel conducting polymer, it is at first synthetic in 1991 by the Bayer company of Germany, poly-ethylenedioxy thiophene (PEDOT) electric conductivity of eigenstate is very poor and water-soluble very poor, but the poly-ethylenedioxy thiophene through overdoping has higher electrical conductivity, and quite stable in air, using kayexalate (PSS) as adulterant and 3, 4-ethylenedioxy thiophene (EDOT) monomer carries out polymerisation, form a kind of Stability Analysis of Structures, poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) aqueous dispersion with high conductance, widened the range of application of the poly-ethylenedioxy thiophene (PEDOT) of conduction, by selecting suitable adulterant or organic solvent, can further regulate electrical conductivity and the water-soluble of PEDOT/PSS, the people such as Dimitriev (Synthetic Metals159 (2009) 2237 – 2239) are by adding ethylene glycol (EG) or dimethyl sulfoxide (DMSO) (DMSO) to improve the electrical conductivity of the PEDOT/PSS film of preparation in PEDOT/PSS solution.method of electrostatic spinning is a kind of method that efficient low-consume prepares nanofiber, in the past few years, by method of electrostatic spinning, prepare the conductive polymer nanometer fiber and obtained remarkable progress, because the strand of most of conducting polymers is rigidity, dissolubility in usual vehicle is very poor, perhaps the viscosity of solution is too low, thereby directly the pure conductive polymer nanometer fiber of electrospinning is generally more difficult, at present, solution mainly contains two kinds, a kind of method is that electrospinning fibre with other macromolecular material is as template, the conducting polymer of in-situ polymerization parcel one deck nanostructured, thereby obtain the conductive polymer micro-nano rice fiber of composite construction, Chinese patent CN201110269757.7 discloses a kind of method for preparing ordered arrangement coaxial configuration electrically conductive polyaniline-polymethyl methacrylate (PANI-PMMA) micro nanometer fiber, another kind method is by nonconducting other polymer (PVAC polyvinylalcohol for example, poly(ethylene oxide) PEO and polymetylmethacrylate) add in the conductive polymer solution that viscosity is very low and increase viscosity, thereby directly the electrospinning composite solution prepares nanofiber, but the method non-conductive polymer material add the electrical conductivity that has reduced composite nano fiber, but Chinese patent CN201310001005 discloses a kind of preparation method of flexibility elongation strain formula sensor, utilize the twist structured PEDOT/PSS micro nanometer fiber of electrospinning process preparation doping polyvinylpyrrolidone PVP, and electric conductivity under its stretching condition is tested, its conductivity at room temperature rate is only 1.6 * 10
-5S cm
-1(Nanoscale, 5 (2013) 7041).ionic liquid (ionic liquid) is that a class presents liquid state in room temperature or near under room temperature, the compound that is formed by zwitterion fully, ionic liquid generally is comprised of organic cation and inorganic or organic anion, existing organic cation comprises the pyridiniujm ion, the imidazole salts ion, quaternary alkylphosphonium salt ion and quaternary ammonium salt ion, inorganic or organic anion comprises halide ion, tetrafluoroborate ion and hexafluorophosphoricacid acid ions, the ionic liquid good conductivity, heat endurance is strong, non-volatile, non-combustible, electrochemical window is large, good in oxidation resistance, be widely applied to electrochemistry, organic synthesis, catalysis with the aspect such as separate, it is a kind of good green solvent.Therefore, seek to provide a kind of preparation technology of conductive-nano-fibers of the ionic liquid that adulterates to have good application prospect.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seek to design the method for poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nanofiber that a kind of electrostatic spinning technique preparation doping ionic liquid is provided, improve electrical conductivity, strengthen the tensile property of nanofiber.
To achieve these goals, the present invention includes precursor spinning solution preparation, nanofiber preparation and three steps of conducting performance test, its specific embodiment is:
(1), precursor spinning solution preparation: be first 2.8% poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) aqueous solution and absolute ethyl alcohol with Dispette to adding respectively mass percent concentration in conical flask, after stirring, polyvinyl alcohol (PVA) is joined in conical flask, heating water bath stirring 1 hour on the magnetic force of routine heating mixer, the solution that obtains is thick black and blue color liquid, the ratio that the solution that then will obtain and ionic liquid 1-ethyl-3-methylimidazole acetate are 30-70:1 according to mass ratio adds ionic liquid 1-ethyl-3-methylimidazole acetate to stir at ambient temperature 1 hour, namely obtain the front body spinning solution of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) of the thick doping ionic liquid of navy blue,
(2), nanofiber preparation: adopt conventional drum-type to collect poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) ordered nano-fibers of electrostatic spinning apparatus preparation doping solion, spinning humidity is not more than 50%, the needle tubing emitter stage internal diameter that drum-type is collected electrostatic spinning apparatus is 0.6 millimeter, distance between needle tubing emitter stage and aluminium foil receiving pole is 7-12 centimetre, and spinning voltage is the 20-24 kilovolt; Poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) ordered nano-fibers of the doping solion that will collect again is wound in poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted that thickness is identical, the diameter of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted is 800 microns, and length is 1.5 centimetres; Poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted sealing that then will prepare saves backup;
(3), conducting performance test: be placed on the silicon substrate of insulation at poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted, the two ends of nano fiber twisted process electrode, with the Pi Anbiao of routine, poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted is carried out to conducting performance test, during test, first on the electrode at nano fiber twisted two ends, add the DC voltage of 5 volts, measure by the electric current of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted, again the resistance of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted under pulled out condition is measured, to gather ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted is fixed on conventional electrically conductive drawn tester, on the electrode at two ends, add 5 volts of DC voltages, nano fiber twisted progressively stretches, electric current reduces gradually, when electric current is little while to unchanged and nano fiber twisted, not being pulled off, stop stretching, record in whole drawing process by the curent change of fiber strands under nanometer, then former length will be recovered after the strand tensile certain-length, after redrawing same length, recover former length, a plurality of circulations so repeatedly, record simultaneously the curent change by nano fiber twisted, test result shows, the room-temperature conductivity of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted of doping ionic liquid 1-ethyl-3-methylimidazole acetate improves an order of magnitude, reaches 10
-4S cm
-1but the recovery stretch rate is 92%.
the mechanism that ionic liquid of the present invention improves poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted electricity and mechanical property is: ionic liquid 1-ethyl-3-methylimidazole acetate is at room temperature the liquid that exists with zwitterion, can as common Bronsted acid, play adulterant, poly-ethylenedioxy thiophene (PEDOT) strand is adulterated, improve electric conductivity, in poly-ethylenedioxy thiophene (PEDOT) molecule, coil conformation and extended conformation coexist, with dipole or the positive charge effect in a polar group in the ionic liquid of a plurality of polar groups and poly-ethylenedioxy thiophene (PEDOT) molecule, another polar group and electronegative kayexalate (PSS) form hydrogen bond, impel the extended conformation of poly-ethylenedioxy thiophene (PEDOT) strand from the coil conformation of low conductivity to high conductivity to change, thereby improve electrical conductivity and the tensile property of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted.
Compared with prior art, its method is simple in the present invention, convenient operation and repetition, and cost is low, and is practical, and electric conductivity and the tensile property of the nanofiber of the doping ionic liquid of preparation are good, are widely used.
The accompanying drawing explanation:
Fig. 1 is the room-temperature conductivity curve map of the PEDOT/PSS nano fiber twisted (doping is 1:33) of the PVA nano fiber twisted of PEDOT/PSS nano fiber twisted, doping ionic liquid of the ionic liquid that do not adulterate that the present invention relates to and doping ionic liquid.
Fig. 2 is the PEDOT/PSS nano fiber twisted electrical conductivity of the doping ionic liquid that the present invention relates to and the graph of relation of tensile elongation.
Fig. 3 be the doping ionic liquid that the present invention relates to the PEDOT/PSS nanofiber repeatedly repeatedly stretch with recover under the conductivity response curve map.
The specific embodiment:
Also the invention will be further described by reference to the accompanying drawings below by embodiment.
Embodiment:
The present embodiment comprises precursor spinning solution preparation, nanofiber preparation and three steps of conducting performance test, and its specific embodiment is:
(1), precursor spinning solution preparation: be first 2.8% poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) aqueous solution and absolute ethyl alcohol with Dispette to adding respectively mass percent concentration in conical flask, after stirring, polyvinyl alcohol (PVA) is joined in conical flask, heating water bath stirring 1 hour on existing magnetic force heating mixer, the solution that obtains is thick black and blue color liquid, the ratio that the solution that then will obtain and ionic liquid 1-ethyl-3-methylimidazole acetate are 30-70:1 according to mass ratio adds ionic liquid 1-ethyl-3-methylimidazole acetate to stir at ambient temperature 1 hour, namely obtain the front body spinning solution of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) of the thick doping ionic liquid of navy blue,
(2), nanofiber preparation: adopt existing drum-type to collect poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) ordered nano-fibers of electrostatic spinning apparatus preparation doping solion, spinning humidity is not more than 50%, the needle tubing emitter stage internal diameter that drum-type is collected electrostatic spinning apparatus is 0.6 millimeter, distance between needle tubing emitter stage and aluminium foil receiving pole is 7-12 centimetre, and spinning voltage is the 20-24 kilovolt; Poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) ordered nano-fibers of the doping solion that will collect again is wound in poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted that thickness is identical, the diameter of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted is 800 microns, and length is 1.5 centimetres; Poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted sealing that then will prepare saves backup;
(3), conducting performance test: be placed on the silicon substrate of insulation at poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted, the two ends of nano fiber twisted process electrode, with Pi Anbiao, poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted is carried out to conducting performance test, during test, first on the electrode at nano fiber twisted two ends, add the DC voltage of 5 volts, measure by the electric current of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted, again the resistance of poly-ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted under pulled out condition is measured, to gather ethylenedioxy thiophene/kayexalate (PEDOT/PSS) nano fiber twisted is fixed on existing electrically conductive drawn tester, on the electrode at two ends, add 5 volts of DC voltages, nano fiber twisted progressively stretches, electric current reduces gradually, when electric current is little while to unchanged and nano fiber twisted, not being pulled off, stop stretching, record in whole drawing process by the curent change of fiber strands under nanometer, then former length will be recovered after the strand tensile certain-length, after redrawing same length, recover former length, a plurality of circulations so repeatedly, record simultaneously the curent change by nano fiber twisted.
The test result of the present embodiment shows: the PEDOT/PSS nano fiber twisted (the doping mass ratio is 1:33) of doping ionic liquid increases by 20 times than the room-temperature conductivity of the nano fiber twisted of the ionic liquid that do not adulterate, and reaches 1.8 * 10
-4S cm
-1And after the doping ionic liquid, the mechanical property of PEDOT/PSS nano fiber twisted is promoted greatly, as shown in table 1, the former long maximum tension rate of recovering of PEDOT/PSS nano fiber twisted of ionic liquid of not adulterating is only 18%, and the recovering former long maximum tension rate and can reach 92% of the PEDOT/PSS twisted wire of doping ionic liquid; Dullness reduces the electrical conductivity of the PEDOT/PSS nano fiber twisted of doping ionic liquid with the increase of tensile elongation, after under certain tensile elongation, through stretching several times, recovering, the current-responsive of twisted wire also tends towards stability, and has good stretching recovery characteristics, can be used for doing strain transducer.
Table 1: the former length of the PEDOT/PSS nano fiber twisted of doping ionic liquid and the ionic liquid that do not adulterate, can recover former long maximal tensility and maximum tension rate
。
Claims (1)
1. the preparation method of ionic liquid conductive-nano-fibers that adulterates, is characterized in that comprising precursor spinning solution preparation, nanofiber preparation and three steps of conducting performance test, and its specific embodiment is:
(1), precursor spinning solution preparation: be first 2.8% the poly-ethylenedioxy thiophene/kayexalate aqueous solution and absolute ethyl alcohol with Dispette to adding respectively mass percent concentration in conical flask, after stirring, polyvinyl alcohol is joined in conical flask, heating water bath stirring 1 hour on the magnetic force of routine heating mixer, the solution that obtains is thick black and blue color liquid, the ratio that the solution that then will obtain and ionic liquid 1-ethyl-3-methylimidazole acetate are 30-70:1 according to mass ratio adds ionic liquid 1-ethyl-3-methylimidazole acetate to stir at ambient temperature 1 hour, namely obtain the front body spinning solution of poly-ethylenedioxy thiophene/kayexalate of the thick doping ionic liquid of navy blue,
(2), nanofiber preparation: adopt conventional drum-type to collect the poly-ethylenedioxy thiophene of electrostatic spinning apparatus preparation doping solion/kayexalate ordered nano-fibers, spinning humidity is not more than 50%, the needle tubing emitter stage internal diameter that drum-type is collected electrostatic spinning apparatus is 0.6 millimeter, distance between needle tubing emitter stage and aluminium foil receiving pole is 7-12 centimetre, and spinning voltage is the 20-24 kilovolt; The poly-ethylenedioxy thiophene of the doping solion that will collect again/kayexalate ordered nano-fibers is wound in the poly-ethylenedioxy thiophene that thickness is identical/kayexalate nano fiber twisted, the diameter of poly-ethylenedioxy thiophene/kayexalate nano fiber twisted is 800 microns, and length is 1.5 centimetres; The poly-ethylenedioxy thiophene that then will prepare/kayexalate nano fiber twisted sealing saves backup;
(3), conducting performance test: be placed on the silicon substrate of insulation at poly-ethylenedioxy thiophene/kayexalate nano fiber twisted, the two ends of nano fiber twisted process electrode, with the Pi Anbiao of routine, poly-ethylenedioxy thiophene/kayexalate nano fiber twisted is carried out to conducting performance test, during test, first on the electrode at nano fiber twisted two ends, add the DC voltage of 5 volts, measure by the electric current of poly-ethylenedioxy thiophene/kayexalate nano fiber twisted, again the resistance of poly-ethylenedioxy thiophene/kayexalate nano fiber twisted under pulled out condition is measured, poly-ethylenedioxy thiophene/kayexalate nano fiber twisted is fixed on conventional electrically conductive drawn tester, on the electrode at two ends, add 5 volts of DC voltages, nano fiber twisted progressively stretches, electric current reduces gradually, when electric current is little while to unchanged and nano fiber twisted, not being pulled off, stop stretching, record in whole drawing process by the curent change of fiber strands under nanometer, then former length will be recovered after the strand tensile certain-length, after redrawing same length, recover former length, a plurality of circulations so repeatedly, record simultaneously the curent change by nano fiber twisted, test result shows, the room-temperature conductivity of the poly-ethylenedioxy thiophene of doping ionic liquid 1-ethyl-3-methylimidazole acetate/kayexalate nano fiber twisted improves an order of magnitude, reaches 10
-4S cm
-1but the recovery stretch rate is 92%.
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| CN104894750A (en) * | 2015-06-16 | 2015-09-09 | 青岛大学 | Force-sensitive stretchable electro-spinning patterning conductive nanofiber membrane and preparation method thereof |
| CN108441287A (en) * | 2018-04-25 | 2018-08-24 | 青岛大学 | A kind of preparation method of the nano combined er materials of Mxene/PS |
| CN110604560A (en) * | 2019-06-19 | 2019-12-24 | 北京大学 | Method for connecting electronic material and hydrogel substrate |
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| CN111850727A (en) * | 2019-04-28 | 2020-10-30 | 合肥杰事杰新材料股份有限公司 | Soft conductor and preparation method thereof |
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| CN111330355B (en) * | 2020-02-28 | 2022-06-14 | 厦门理工学院 | Electret nanofiber high-efficiency filter material and preparation method thereof |
| CN111876845A (en) * | 2020-08-05 | 2020-11-03 | 扬州大学 | Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof |
| CN111876845B (en) * | 2020-08-05 | 2022-12-02 | 扬州大学 | Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof |
| CN113638128A (en) * | 2021-08-13 | 2021-11-12 | 大连理工大学 | Preparation method of thin film material capable of realizing temperature and strain dual-function self-driven sensing |
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Application publication date: 20131120 |