CN111876845B - Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof - Google Patents

Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof Download PDF

Info

Publication number
CN111876845B
CN111876845B CN202010777077.5A CN202010777077A CN111876845B CN 111876845 B CN111876845 B CN 111876845B CN 202010777077 A CN202010777077 A CN 202010777077A CN 111876845 B CN111876845 B CN 111876845B
Authority
CN
China
Prior art keywords
pedot
pss
array structure
fiber
spinning
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202010777077.5A
Other languages
Chinese (zh)
Other versions
CN111876845A (en
Inventor
高强
王鹏
沈明
高春霞
王明序
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yangzhou University
Original Assignee
Yangzhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yangzhou University filed Critical Yangzhou University
Priority to CN202010777077.5A priority Critical patent/CN111876845B/en
Publication of CN111876845A publication Critical patent/CN111876845A/en
Application granted granted Critical
Publication of CN111876845B publication Critical patent/CN111876845B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D01D5/36—Matrix structure; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
  • Multicomponent Fibers (AREA)

Abstract

The invention relates to a spinning method of PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) conductive fibers with a surface array structure and conductive fibers thereof in the technical field of conductive fiber preparation, and particularly relates to a spinning method of PEDOT/PSS conductive fibers with a surface array structure and conductive fibers thereof, wherein a prepared PEDOT/PSS spinning solution enters a mixed coagulating bath of ethanol and water through a wet spinning spinneret for coagulation forming, and 0.1-0.5 mol/L soluble Cu is added into the mixed coagulating bath of the ethanol and the water 2+ And drawing, drying and cooling the solidified and formed fiber, and standing in air at room temperature until the array structure on the surface of the fiber is self-assembled to obtain the high-conductivity PEDOT (Poly ethylene glycol ether ketone) (PSS) conductive fiber with the surface array structure. In the spinning method of the present invention, cu is added to the coagulation bath 2+ The continuous PEDOT PSS conductive fiber with the surface array structure can be simply and efficiently prepared. The array structure can remarkably increase the specific surface area of the fiber, provides more active sites for post-treatment such as fiber surface grafting and the like, has better sensing performance on air flow, touch pressure and the like, and is more favorable for being applied to aspects such as flexible sensors and the like.

Description

Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof
Technical Field
The invention relates to the technical field of preparation of organic polymer conductive fibers, in particular to a spinning method of PEDOT (PolyEthylenediamine) PSS (PolyEthylenediamine) conductive fibers with a surface array structure and conductive fibers thereof.
Background
The poly 3,4-ethylenedioxythiophene (PEDOT) is a polymer of EDOT monomers, a thiophene ring on a main chain enables PEDOT molecular chains to show stronger rigidity and be insoluble in general organic solvents, and after the poly (ethylene terephthalate sulfonate) anion (PSS) is doped, uniform and stable dispersion of PEDOT: PSS aqueous dispersion can be obtained. The PEDOT PSS material has high conductivity and good optical transparency. Under proper conditions, the continuous fiber can be prepared by a relatively simple wet spinning technology, and has wide application prospect in the aspect of electronic textile products. However, the usually prepared PEDOT/PSS fiber has smooth surface and small specific surface area, and after the PSS component is removed by washing with dimethyl sulfoxide, ethylene glycol, sorbitol and the like, although the conductivity can be greatly improved, the number of active sites on the fiber surface is also sharply reduced, so that the application of the PEDOT/PSS fiber is limited. Therefore, how to simply and efficiently prepare the PEDOT/PSS conductive fiber with large specific surface area, many active sites, strong continuity and high conductivity becomes a popular research subject at home and abroad.
At present, researches on improving the specific surface area of PEDOT/PSS conductive fibers mainly comprise that PEDOT/PSS dispersion liquid and small molecules are subjected to composite spinning, and the surfaces of the fibers are subjected to high wrinkling by a method for removing the small molecules, or nanoparticles are deposited on the surfaces of the fibers to obtain the fibers with high specific surface areas. The research for improving the active sites on the surface of the fiber is mostly to obtain the PEDOT: PSS fiber with more active sites by compositely spinning the PEDOT: PSS dispersion liquid and a high-activity substance. These methods are often cumbersome to operate and increase the cost of the process.
By adding Cu to a coagulation bath consisting of ethanol and water 2+ No related research on preparing the PEDOT/PSS conductive fiber with the surface regular array structure by a one-step method is reported at present.
Disclosure of Invention
Aiming at the problems of complicated operation and high cost of the process method for improving the specific surface area of the PEDOT/PSS conductive fiber in the prior art, the invention provides the spinning method of the PEDOT/PSS conductive fiber with the surface array structure, which adds soluble Cu into a mixed coagulating bath consisting of ethanol and water in the wet spinning process 2+ The surface of the auxiliary fiber forms a regularly arranged array structure to improve the specific surface area of the fiber and the electrical conductivity of the fiberRate and overall performance.
The invention aims to realize a spinning method of PEDOT: PSS conductive fibers with a surface array structure, which is characterized by comprising the following steps:
the first step is as follows: preparing PEDOT, namely PSS spinning solution;
the second step is that: feeding the spinning solution into a mixed coagulating bath of ethanol and water through a wet spinning spinneret for coagulation forming, wherein 0.1-0.5 mol/L soluble Cu is added into the mixed coagulating bath of the ethanol and the water 2+ And drawing, drying and cooling the solidified and formed fiber, and standing in air at room temperature for 12-60 h to prepare the PEDOT/PSS conductive fiber with the surface array structure.
In the spinning method of the present invention, cu is added to an ethanol/water coagulation bath 2+ PSS conductive fiber with a surface array structure is simply and efficiently obtained by the limited-area self-assembly of the PSS-Cu complex on the surface of the PEDOT fiber in the one-step wet spinning process, so that the conductive fiber is more favorable for being applied to the aspect of flexible sensors, and meanwhile, the conductivity of the fiber is obviously improved by the doping of copper ions, and unexpected technical effects are obtained. In addition, in the spinning method, the used coagulating bath is ethanol and water, so that the spinning method is green, environment-friendly, non-toxic and harmless; the added soluble copper ions have low concentration and small dosage, and are suitable for large-scale industrial production.
Preferably, in the first step, the PEDOT/PSS spinning solution is prepared by shaking a PEDOT/PSS aqueous dispersion solution for 5-30 min by an ultrasonic oscillator, uniformly mixing, standing and defoaming.
Furthermore, the dispersion concentration of PEDOT, PSS is 15-25 mg/mL; the working frequency of the ultrasonic oscillator is 30-60 KHz.
As the coagulation bath in the present invention, preferably, in the second step, the volume ratio of ethanol and water in the mixed coagulation bath is: (1-5): 1.
In a further preferred embodiment of the invention, in the second step, the soluble Cu is 2+ By CuCl 2 And (4) adding.
Further, in the second step, the aperture of the spinneret is 0.13-0.51 mm.
Further, in the second step, the fiber drawing method after coagulation forming in the coagulation bath is: and fishing out the fiber when the fiber reaches the bottom of the coagulating bath, drying and cooling the fiber, and winding the fiber to the periphery of a polytetrafluoroethylene rod or a roller.
By adding Cu to an ethanol/water coagulation bath as described above 2+ The invention also provides a PEDOT PSS conductive fiber with a surface array structure. The conductive fiber has a regular array structure, the specific surface area of the fiber is obviously increased, more active sites are provided for post-treatment such as fiber surface grafting, and the like, and the conductive fiber has better sensing performance on air flow, touch pressure and the like, and is more favorable for being applied to aspects such as flexible sensors and the like.
Drawings
FIG. 1 shows 25 mg/ml PEDOT PSS dope in CuCl 2 SEM image of wet spun fibers in a mixed coagulation bath of ethanol/water at a molar concentration of 0.4 mol/L at a ratio of 1: 1;
FIG. 2 shows 18 mg/ml PEDOT PSS spin dope in CuCl 2 SEM image of wet spun fibers in 5: 1 mixed coagulation bath of ethanol/water with 0.2 mol/L molarity;
FIG. 3 shows 20 mg/ml PEDOT PSS spin dope in CuCl 2 SEM image of wet spun fibers in a mixed coagulation bath of ethanol/water 3: 1 with a molar concentration of 0.1 mol/L;
FIG. 4 shows 15 mg/ml PEDOT PSS spin dope in CuCl 2 SEM image of wet spun fibers in a mixed coagulation bath with a molar concentration of 0.5 mol/L ethanol/water at 2: 1;
FIG. 5 shows 20 mg/ml PEDOT: PSS spin dope in CuCl 2 SEM image of wet spun fibers in a 3: 1 mixed coagulation bath with 0.05 mol/L ethanol/water molar concentration;
FIG. 6 shows 20 mg/ml PEDOT PSS spin dope in CaCl 2 SEM image of wet spun fibers in a mixed coagulation bath of ethanol/water 3: 1 with a molar concentration of 0.1 mol/L;
FIG. 7 shows 20 mg/ml PEDOT PSS spin dope in ZnCl 2 SEM image of wet spun fibers in a mixed coagulation bath with a molar concentration of 0.1 mol/L ethanol/water 3: 1;
FIG. 8 is an SEM image of 20 mg/ml PEDOT: PSS spin dope wet spun fibers in a mixed coagulation bath with KCl molar concentration of 0.1 mol/L ethanol/water 3: 1;
FIG. 9 is a graph of conductivity of PEDOT PSS fibers in various examples and comparative examples.
Detailed Description
The following examples are intended to simulate the spinning process of the present invention in order to facilitate the detailed description of the invention, and it is necessary to point out here that the following examples are intended only to illustrate the invention and should not be interpreted as limiting the scope of protection of the invention. It will be understood that various changes and modifications can be made by one skilled in the art after reading the present invention, and equivalents fall within the scope of the invention as defined by the appended claims.
Example 1
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating a PEDOT (Polytetrafluoroethylene) PSS aqueous dispersion to 25 mg/ml by using a heating stirrer, placing the dispersion in an ultrasonic oscillator with the working frequency of 35 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing, defoaming, and then putting into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.25 mm;
then, a coagulation bath was prepared: the coagulation bath in this example was made of ethanol, water and CuCl 2 The volume ratio of ethanol to water is 1: 1; cuCl 2 The concentration of (2) added was 0.4 mol/L. Firstly, cuCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding the PEDOT (PSS) spinning solution at a constant speed, wherein the advancing speed is 20 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the self-assembly of the fiber surface array structure is finished. The SEM image of the PEDOT PSS conductive fiber spun by the embodiment is shown in figure 1, and the surface of the fiber has a regular array structure. The conductivity was 7.31S/cm as shown in FIG. 9.
Example 2
Firstly, preparing PEDOT, PSS spinning solution: concentrating a PEDOT (Polytetrafluoroethylene) PSS aqueous dispersion to 18 mg/ml by using a heating stirrer, placing the dispersion in an ultrasonic oscillator with the working frequency of 45 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing, defoaming, and then filling into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.25 mm;
then, a coagulation bath was prepared: the coagulation bath in this example was made of ethanol, water and CuCl 2 The volume ratio of ethanol to water is 5: 1; cuCl 2 The concentration of (2) added was 0.2 mol/L. Firstly, cuCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding the PEDOT (PSS) spinning solution at a constant speed, wherein the advancing speed is 30 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the array structure on the surface of the fibers is self-assembled. PSS conductive fiber, the SEM image of which is shown in FIG. 2, of PEDOT spun in this example, the surface of the fiber has a regular array structure, and the conductivity of the fiber is 3.46S/cm, as shown in FIG. 9.
Example 3
Firstly, preparing PEDOT, PSS spinning solution: concentrating the PEDOT: PSS aqueous dispersion to 20 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 45 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.33 mm;
then, a coagulation bath was prepared: the coagulation bath in this example was made of ethanol, water and CuCl 2 The volume ratio of ethanol to water is 3: 1; cuCl 2 The concentration of (2) added was 0.1 mol/L. Firstly, cuCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding the PEDOT (PSS) spinning solution at a constant speed, wherein the advancing speed is 20 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the self-assembly of the fiber surface array structure is finished. PSS conductive fiber, the SEM image of the conductive fiber spun by the embodiment is shown in figure 3, the surface of the fiber has a regular array structure, and the conductivity of the conductive fiber is 4.27S/cm, as shown in figure 9.
Example 4
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating a PEDOT (Polytetrafluoroethylene) PSS aqueous dispersion to 15 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 60 KHz for ultrasonic oscillation for 15 min to form a uniformly dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.5 mm;
then, a coagulation bath was prepared: the coagulating bath in this embodiment is composed of ethanol, water and CuCl 2 The volume ratio of ethanol to water is 2: 1; cuCl 2 The concentration of (2) added was 0.5 mol/L. Firstly, cuCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding a PEDOT (Polytetrafluoroethylene) spinning solution at a constant speed, wherein the advancing speed is 15 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the array structure on the surface of the fibers is self-assembled. PSS conductive fiber, the SEM image of the conductive fiber spun by the embodiment is shown in figure 4, the surface of the fiber has a regular array structure, and the conductivity of the conductive fiber is 2.74S/cm, as shown in figure 9.
Comparative example 1
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating the PEDOT: PSS aqueous dispersion to 20 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 45 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.33 mm;
then, a coagulation bath was prepared: the coagulation bath in this comparative example was made of ethanol, water and CuCl 2 The volume ratio of ethanol to water is 3: 1; cuCl 2 The concentration of (2) was 0.05 mol/L. Firstly, cuCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding a PEDOT (Polytetrafluoroethylene) spinning solution at a constant speed, wherein the advancing speed is 20 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the array structure on the surface of the fibers is self-assembled. PSS conductive fiber, the SEM image of which is shown in FIG. 5, has a small amount of fine particles on the surface, can not form a regular array structure, and the conductivity of which is 0.93S/cm, as shown in FIG. 9.
Comparative example 2
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating a PEDOT (Polytetrafluoroethylene) PSS aqueous dispersion to 20 mg/ml by using a heating stirrer, placing the dispersion in an ultrasonic oscillator with the working frequency of 45 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing, defoaming, and then putting into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.33 mm;
then, a coagulation bath was prepared: the coagulation bath in this comparative example was made of ethanol, water and CaCl 2 The volume ratio of ethanol to water is 3: 1; caCl 2 The concentration of (2) added was 0.1 mol/L. Firstly, caCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding a PEDOT (Polytetrafluoroethylene) spinning solution at a constant speed, wherein the advancing speed is 20 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the array structure on the surface of the fibers is self-assembled. PSS conductive fiber SEM picture that this comparative example spun PEDOT, the fiber surface was rough, but there was no regular array structure, the conductivity was 0.06S/cm, as shown in FIG. 9.
Comparative example 3
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating a PEDOT (Polytetrafluoroethylene) PSS aqueous dispersion to 20 mg/ml by using a heating stirrer, placing the dispersion in an ultrasonic oscillator with the working frequency of 45 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing, defoaming, and then putting into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.33 mm;
then, a coagulation bath was prepared: the coagulation bath in this comparative example was composed of ethanol, water and ZnCl 2 The proportion of the ethanol and the water is 3: 1; znCl 2 The concentration of (2) added was 0.1 mol/L. Firstly ZnCl is added 2 Dissolving in water, adding ethanol, and stirring;
and finally, wet spinning: and extruding a PEDOT (Polytetrafluoroethylene) spinning solution at a constant speed, wherein the advancing speed is 20 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the array structure on the surface of the fibers is self-assembled. PSS conductive fiber SEM picture that this comparative example spun PEDOT, the fiber surface was smooth, there was no regular array structure, its conductivity was 0.74S/cm, as shown in FIG. 9.
Comparative example 4
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating a PEDOT (Polytetrafluoroethylene) PSS aqueous dispersion to 20 mg/ml by using a heating stirrer, placing the dispersion in an ultrasonic oscillator with the working frequency of 45 KHz for ultrasonic oscillation for 15 min to form uniformly dispersed spinning solution, standing, defoaming, and then putting into a spinning solution storage tank, wherein the pore diameter of a spinneret plate is 0.33 mm;
then, a coagulation bath was prepared: the coagulation bath in this comparative example was a mixed solution consisting of ethanol, water and KCl, the ratio of ethanol to water being 3: 1; the addition concentration of KCl is 0.1 mol/L, KCl is dissolved in water, ethanol is added, and the mixture is fully and uniformly stirred for later use;
and finally, wet spinning: and extruding the PEDOT (PSS) spinning solution at a constant speed, wherein the propelling speed is 5 ml/h, fishing out the extruded fibers when the extruded fibers reach the bottom of a coagulating bath, drying the extruded fibers by a drying lamp, winding and collecting the extruded fibers by a polytetrafluoroethylene roller, standing the extruded fibers in the air at room temperature, and sealing and storing the extruded fibers after the self-assembly of the fiber surface array structure is finished. PSS conductive fiber SEM picture that this comparative example spun PEDOT, the fiber surface was smooth, there was no regular array structure, its conductivity was 0.67S/cm, as shown in FIG. 9.

Claims (7)

1. The spinning method of the PEDOT PSS conductive fiber with the surface array structure is characterized by comprising the following steps of:
the first step is as follows: preparing PEDOT, namely PSS spinning solution;
the second step is that: the spinning solution enters a mixed coagulation bath of ethanol and water for coagulation forming through a wet spinning spinneret, the volume ratio of the ethanol to the water is (1-5): 1, and 0.1-0.5 mol/L soluble Cu is added into the mixed coagulation bath 2+ And drawing, drying and cooling the solidified and formed fiber, and standing in air at room temperature until the array structure on the surface of the fiber is self-assembled to obtain the PEDOT/PSS conductive fiber with the surface array structure.
2. The spinning method of the PEDOT PSS conductive fiber with the surface array structure according to claim 1, wherein in the first step, the PEDOT PSS spinning solution is at normal temperature, the PEDOT PSS water dispersion is vibrated for 5-30 min by an ultrasonic oscillator, and the uniform spinning solution is prepared by standing and defoaming after uniform mixing.
3. The spinning method of the PEDOT PSS conductive fiber with the surface array structure as claimed in claim 2, wherein the concentration of the dispersion of the PEDOT PSS is 15-25 mg/mL; the working frequency of the ultrasonic oscillator is 30-60 KHz.
4. PSS conductive PEDOT fiber spinning method with surface array structure as claimed in claim 1, characterized in that in the second step soluble Cu 2+ By CuCl 2 And (4) adding.
5. PSS conductive fiber spinning method according to claim 1, characterized in that in the second step, the aperture of the spinneret is 0.13-0.51 mm.
6. PSS conductive fiber spinning method of PEDOT with surface array structure as claimed in claim 1, characterized in that in the second step, the fiber drawing method after coagulation formation in coagulation bath is: and fishing out the fibers when the fibers reach the bottom of the coagulating bath, drying and cooling the fibers, and winding the fibers to the periphery of a polytetrafluoroethylene rod or a roller.
7. PSS conductive PEDOT fibers having a surface array structure, characterized in that they are spun by a spinning process according to any one of claims 1 to 6.
CN202010777077.5A 2020-08-05 2020-08-05 Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof Active CN111876845B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010777077.5A CN111876845B (en) 2020-08-05 2020-08-05 Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010777077.5A CN111876845B (en) 2020-08-05 2020-08-05 Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof

Publications (2)

Publication Number Publication Date
CN111876845A CN111876845A (en) 2020-11-03
CN111876845B true CN111876845B (en) 2022-12-02

Family

ID=73211708

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010777077.5A Active CN111876845B (en) 2020-08-05 2020-08-05 Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof

Country Status (1)

Country Link
CN (1) CN111876845B (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103397402A (en) * 2013-07-23 2013-11-20 青岛大学 Preparation method of ionic liquid-doped conductive nanofiber
CN106381571A (en) * 2016-08-25 2017-02-08 中国工程物理研究院化工材料研究所 PEDOT:PSS fiber and preparation method thereof
CN109295707A (en) * 2018-10-10 2019-02-01 东华大学 A kind of flexible thermal conducting nanofiber film and its preparation and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103397402A (en) * 2013-07-23 2013-11-20 青岛大学 Preparation method of ionic liquid-doped conductive nanofiber
CN106381571A (en) * 2016-08-25 2017-02-08 中国工程物理研究院化工材料研究所 PEDOT:PSS fiber and preparation method thereof
CN109295707A (en) * 2018-10-10 2019-02-01 东华大学 A kind of flexible thermal conducting nanofiber film and its preparation and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Anion effect on salt-induced conductivity enhancement of poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) films;Xia, Yijie et al.;《Organic Electronics》;ELSEVIER;20100630;第11卷(第6期);第1130-1134页，第1节 最后一段，第2节 倒数第二段，第3.1节 最后一段，表格1中内容 *

Also Published As

Publication number Publication date
CN111876845A (en) 2020-11-03

Similar Documents

Publication Publication Date Title
Bavatharani et al. Electrospinning technique for production of polyaniline nanocomposites/nanofibres for multi-functional applications: A review
CN111793853B (en) Spinning method of PEDOT (polyethylene glycol terephthalate): PSS (Poly styrene) conductive fiber with high elongation
Wang et al. Conductive polymer ultrafine fibers via electrospinning: Preparation, physical properties and applications
CN114108132B (en) Preparation method of high-strength high-conductivity PEDOT fiber
CN101585907B (en) Preparation method of conductive polymer poly (3, 4-ethylenedioxythiophene) hollow microspheres
CN103408754B (en) A kind of preparation method of polyaniline nano fiber
CN110387743B (en) Conductive composite fiber bundle and preparation method thereof
CN104963098A (en) Method for preparing electrostatic spinning perfluocarbon polymer nanofiber membrane
CN1710160A (en) Method for preparing meta aromatic polyamide fiber
CN106012086A (en) Graphene/polyaniline composite fiber and preparation method thereof
CN109537083A (en) A kind of preparation method and applications of graphene/polyaniline nano-composite fiber film
CN101710541B (en) Preparation method of polyaniline nano-fiber electrode material for super capacitor
CN111876845B (en) Spinning method of PEDOT (Polytetrafluoroethylene-PSS) conductive fiber with surface array structure and conductive fiber thereof
CN115679468A (en) Preparation method of hollow PEDOT (PEDOT-PSS) fiber
CN102161092B (en) Nano silver capable of being dispersed in hydrophilic system and preparation method thereof
CN100412110C (en) Polyaniline nano fiber and its preparing process
CN102875978A (en) Preparation method of gold nanoparticle/poly (3, 4-dioxyethyl) thiophene composite material
CN101864082A (en) Preparation method of chitin film
CN109273271B (en) High-conductivity flexible self-supporting all-solid-state supercapacitor and preparation method thereof
CN104451931A (en) Method for preparing rare earth polysaccharide composite fibers
Wang et al. Polypyrrole micro/nanostructures and their soft materials in versatile forms: construction and applications
CN108314780B (en) A kind of preparation method of highly conductive poly- 3,4- ethylenedioxy thiophene porous electrode material
CN106496528A (en) A kind of method that utilization micro passage reaction prepares PEDOT PSS aqueous liquid dispersions
CN116288797A (en) Flexible PEDOT (polyether-ether-ketone) PSS (power supply system) conductive composite fiber and preparation method thereof
CN110010368A (en) A kind of poly- 3,4- ethylenedioxy thiophene of sheet and the preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant