CN111793853B - Spinning method of PEDOT (polyethylene glycol terephthalate): PSS (Poly styrene) conductive fiber with high elongation - Google Patents

Spinning method of PEDOT (polyethylene glycol terephthalate): PSS (Poly styrene) conductive fiber with high elongation Download PDF

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CN111793853B
CN111793853B CN202010777076.0A CN202010777076A CN111793853B CN 111793853 B CN111793853 B CN 111793853B CN 202010777076 A CN202010777076 A CN 202010777076A CN 111793853 B CN111793853 B CN 111793853B
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pedot
pss
fiber
spinning
water
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CN111793853A (en
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高强
王鹏
沈明
高春霞
冯丹洋
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Yangzhou University
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    • 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
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • 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

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

Abstract

The invention relates to a wet spinning method of PEDOT (PolyEthylenediamine) PSS (PolyEthylenediamine) conductive fiber with high elongation in the preparation technology of organic polymer conductive fiber, which comprises the following steps: firstly, preparing PEDOT, namely PSS spinning solution; then, allowing the spinning solution to enter a mixed coagulating bath of ethanol and water through a wet spinning spinneret for coagulation forming, wherein LiCl is added into the mixed coagulating bath of ethanol and water, and the addition concentration is 0.1-0.5 mol/L; and drawing, drying and cooling the solidified and formed fiber to prepare the PEDOT (PSS) conductive fiber with high conductivity and high elongation. The method adopts a one-step wet spinning method, adopts a water/ethanol system coagulation bath as a main body, and adds lithium ions in the coagulation bath to assist the solidification and molding of the fiber, so that the tensile elongation and the conductivity of the fiber are obviously improved, and the application range and the processing adaptability of the fiber in textile materials are expanded.

Description

Spinning method of PEDOT (Polytetrafluoroethylene)/PSS (Polytetrafluoroethylene) conductive fiber with high elongation
Technical Field
The invention relates to the technical field of preparation of organic polymer conductive fibers, in particular to a spinning method of PEDOT (PolyEthylenedimethylene terephthalate) -PSS (PolyEthylenedimethylene terephthalate) conductive fibers with high elongation.
Background
Poly 3, 4-ethylenedioxythiophene (PEDOT) is a prototype conjugated polymer used as a hole injection/transport layer in organic (opto) electronic devices in a doped state, which, after doping with poly (styrene sulfonate anion) (PSS), gives a homogeneously dispersed and stable aqueous suspension of PEDOT: PSS, which has both 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, PEDOT PSS fiber has poor stretchability and cannot meet the processing requirements of some textile materials. Therefore, how to simply and efficiently prepare the PEDOT/PSS conductive fiber with strong continuity and high elongation rate becomes a popular topic at home and abroad.
At present, researches for improving the tensile elongation of PEDOT and PSS conductive fibers mainly comprise mixing and spinning high-flexibility water-soluble polymers such as PEDOT, PSS and PVA, or changing the concentration of PEDOT and PSS spinning solution. The methods are all based on an organic coagulating bath system of acetone/isopropanol, the coagulating bath has a strong phase separation effect on PSS dispersion, and the diffusion and exchange processes between the two components are too rapid, so that wet-formed PEDOT (PSS fiber) is crisp and hard in hand feeling (the elongation is low, about 5-12%), and the flexibility advantage of the fiber cannot be completely reflected. If the conductivity of the fiber is improved by removing the residual PSS in the obtained fiber by washing with dimethyl sulfoxide, ethylene glycol, or the like during the post-treatment of the fiber, the stretchability of the fiber is further reduced. Acetone and isopropanol are toxic to human bodies, the coagulating bath is expensive, and environmental pollution is easy to cause. The water and the ethanol related to the invention belong to conventional reagents, are safe and nontoxic, have wide sources and are easy to obtain, and the spinning cost is also reduced.
Disclosure of Invention
The invention aims to provide a wet spinning method of PEDOT/PSS conductive fibers with high conductivity and high elongation, which has the advantages of simple preparation process, low cost and good comprehensive performance, so as to simplify the spinning process and reduce the spinning cost.
The invention aims to realize a spinning method of PEDOT: PSS conductive fibers with high elongation, which is characterized by comprising the following steps:
the first step is as follows: preparing PEDOT, namely PSS spinning solution;
the second step: enabling the spinning solution to enter a mixed coagulating bath of ethanol and water through a wet spinning spinneret for coagulation forming, wherein LiCl is added into the mixed coagulating bath of the ethanol and the water, and the adding concentration is 0.1-0.5 mol/L; and drawing, drying and cooling the solidified and formed fiber to obtain the PEDOT/PSS conductive fiber with high conductivity and high elongation.
The method adopts one-step wet spinning, adopts a water/ethanol system coagulating bath as a main body, and adds lithium ions in the coagulating bath to assist the solidification and molding of the fiber, so that the lithium ions are doped in the fiber, the tensile elongation and the conductivity of the fiber are obviously improved, and the application range and the processing adaptability of the fiber in textile materials are expanded.
Further, in the first step, the PEDOT/PSS spinning solution is vibrated for 5-30 min by an ultrasonic oscillator at normal temperature, and is mixed uniformly and then is kept stand for deaeration to prepare the uniform spinning solution.
Furthermore, the water dispersion concentration of PEDOT to PSS is 15-25 mg/mL; the working frequency of the ultrasonic oscillator is 30-60 KHz.
Further, in the second step, the volume ratio of ethanol to water in the mixed coagulation bath is: (2-5): 1.
Furthermore, in the second step, the aperture of a spinneret plate for spraying the spinning solution is 0.13-0.51 mm.
In order to facilitate drawing of the fiber, in the second step, the drawing method of the fiber after coagulation forming in the coagulation bath is as follows: and fishing out the fiber when the fiber reaches the bottom of the coagulating bath, and winding the fiber to the periphery of a polytetrafluoroethylene rod or a roller.
Drawings
FIG. 1 is a stress-strain curve of 25 mg/ml PEDOT: PSS dope wet spun fiber in a mixed coagulation bath of 0.1 mol/L LiCl in ethanol/water 3: 1;
FIG. 2 is a stress-strain curve of 23 mg/ml PEDOT: PSS spinning dope wet spinning fibers in a mixed coagulation bath of 0.1 mol/L LiCl in ethanol/water at a ratio of 2: 1;
FIG. 3 is a stress-strain curve of 20 mg/ml PEDOT: PSS dope wet spun fiber in a mixed coagulation bath of 0.1 mol/L LiCl in 5: 1 ethanol/water;
FIG. 4 is a stress-strain curve of 20 mg/ml PEDOT: PSS dope wet spun fiber in a mixed coagulation bath of 0.5 mol/L LiCl in ethanol/water at a ratio of 3: 1;
FIG. 5 is a stress-strain curve of 25 mg/ml PEDOT: PSS dope wet spun fiber in a mixed coagulation bath of 0.06 mol/L LiCl in ethanol/water 3: 1;
FIG. 6 shows 23 mg/ml PEDOT PSS dope in CaCl 2 Stress-strain curve of wet-spun fibers in a 2: 1 mixed coagulation bath with 0.1 mol/L ethanol/water molar concentration;
FIG. 7 is a stress-strain curve of 20 mg/ml PEDOT: PSS dope wet spun fiber in a mixed coagulation bath of KCl molar concentration 0.1 mol/L ethanol/water 5: 1;
FIG. 8 is a stress-strain curve of 20 mg/ml PEDOT: PSS dope wet spun fiber in a mixed coagulation bath of 0.1 mol/L LiCl in ethanol/water at 1: 0;
FIG. 9 is a graph of conductivity of PEDOT PSS fibers of various examples and comparative examples.
Detailed Description
The following examples, which are intended to illustrate the invention and not to limit its scope, are given by way of illustration only, and it is to be understood that various changes and modifications may be made by one skilled in the art after reading the present disclosure and that equivalents may be made thereto without departing from the scope of the invention as defined in the appended claims.
Example 1
Firstly, preparing PEDOT, PSS spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 25 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 35 KHz for ultrasonic oscillation for 15 min to form uniform and dispersed spinning solution, standing for defoaming, and then placing the spinning solution into a spinning solution storage tank, wherein the aperture of a spinneret plate is 0.25 mm;
then, preparing a coagulating bath, wherein the coagulating bath in the embodiment is a mixed solution consisting of ethanol, water and LiCl, and the volume ratio of the ethanol to the water is 3: 1; the LiCl was added at a concentration of 0.1 mol/L. Firstly, dissolving LiCl in water, then adding ethanol, and fully and uniformly stirring for later use;
and finally, wet spinning: and extruding the PEDOT PSS spinning solution at a constant speed, wherein the advancing speed is 5 ml/h, fishing out the extruded fiber when the extruded fiber reaches the bottom of a coagulating bath, drying by a drying lamp, and winding and collecting by a polytetrafluoroethylene roller to obtain the PEDOT PSS conductive fiber with high tensile elongation of the embodiment. The stress-strain curve of the PEDOT PSS conductive fiber spun in this example is shown in FIG. 1, and the tensile elongation is 55.0%. The conductivity was 3.65S/cm, as shown in FIG. 9.
Example 2
Firstly, preparing PEDOT, PSS spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 23 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 50 KHz for ultrasonic oscillation for 15 min to form uniform dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the aperture of a spinneret plate is 0.25 mm;
then, preparing a coagulating bath, wherein the coagulating bath in the embodiment is a mixed solution consisting of ethanol, water and LiCl, and the volume ratio of the ethanol to the water is 2: 1; the LiCl was added at a concentration of 0.1 mol/L. Firstly, dissolving LiCl in water, adding ethanol, and fully and uniformly stirring for later use;
and finally, wet spinning: and extruding the PEDOT PSS spinning solution at a constant speed, wherein the advancing speed is 10 ml/h, fishing out the extruded fiber when the extruded fiber reaches the bottom of a coagulating bath, drying by a baking lamp, and winding and collecting by a polytetrafluoroethylene roller to obtain the PEDOT PSS conductive fiber with high tensile elongation. The stress-strain curve of the PEDOT PSS conductive fiber spun in this example is shown in FIG. 2, the tensile elongation is 51.9%, and the electrical conductivity is 5.95S/cm, as shown in FIG. 9.
Example 3
Firstly, preparing PEDOT, PSS spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 20 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 uniform dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the aperture of a spinneret plate is 0.33 mm;
then, preparing a coagulating bath, wherein the coagulating bath in the embodiment is a mixed solution consisting of ethanol, water and LiCl, and the volume ratio of the ethanol to the water is 5: 1; the LiCl was added at a concentration of 0.1 mol/L. Firstly, dissolving LiCl in water, adding ethanol, and fully and uniformly stirring for later use;
and finally, wet spinning: and extruding the PEDOT PSS spinning solution at a constant speed, wherein the advancing speed is 5 ml/h, fishing out the extruded fiber when the extruded fiber reaches the bottom of a coagulating bath, drying by a drying lamp, and winding and collecting by a polytetrafluoroethylene roller to obtain the PEDOT PSS conductive fiber with high tensile elongation of the embodiment. The stress-strain curve of the PEDOT PSS conductive fiber spun in this example is shown in FIG. 3, the tensile elongation is 51.1%, and the electrical conductivity is 2.98S/cm, as shown in FIG. 9.
Example 4
Firstly, preparing PEDOT, PSS spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 20 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 50 KHz for ultrasonic oscillation for 15 min to form uniform dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the aperture of a spinneret plate is 0.33 mm;
then, preparing a coagulating bath, wherein the coagulating bath in the embodiment is a mixed solution consisting of ethanol, water and LiCl, and the volume ratio of the ethanol to the water is 3: 1; the LiCl was added at a concentration of 0.5 mol/L. Firstly, dissolving LiCl in water, adding ethanol, and fully and uniformly stirring for later use;
and finally, wet spinning: and extruding the PEDOT PSS spinning solution at a constant speed, wherein the advancing speed is 5 ml/h, fishing out the extruded fiber when the extruded fiber reaches the bottom of a coagulating bath, drying by a baking lamp, and winding and collecting by a polytetrafluoroethylene roller to obtain the PEDOT PSS conductive fiber with high tensile elongation. The stress-strain curve of the PEDOT PSS conductive fiber spun in this example is shown in FIG. 4, the tensile elongation is 50%, and the electrical conductivity is 1.23S/cm, as shown in FIG. 9.
Comparative example 1
Firstly, preparing PEDOT, PSS spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 25 mg/ml by using a heating stirrer, then placing the dispersion in an ultrasonic oscillator with the working frequency of 35 KHz for ultrasonic oscillation for 15 min to form uniform and dispersed spinning solution, standing for defoaming, and then placing the spinning solution into a spinning solution storage tank, wherein the aperture of a spinneret plate is 0.25 mm;
then, a coagulation bath was prepared: the coagulation bath in the comparative example was a mixed solution consisting of ethanol, water and LiCl, the volume ratio of ethanol to water being 3: 1; the LiCl was added at a concentration of 0.06 mol/L. Firstly, dissolving LiCl in water, then adding ethanol and fully stirring for later use;
and finally, wet spinning: and extruding the PEDOT PSS spinning solution at a constant speed, wherein the advancing 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, and collecting the fibers by a polytetrafluoroethylene roller. PSS fiber spun from this comparative example had a stress-strain curve as shown in FIG. 5, a tensile elongation of 21.2%, and an electrical conductivity of 2.21S/cm as shown in FIG. 9.
Comparative example 2
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: PSS water dispersion of PEDOT is concentrated to 23 mg/ml by a heating stirrer, then the dispersion is placed in an ultrasonic oscillator with the working frequency of 50 KHz for ultrasonic oscillation for 15 min, so that uniform dispersed spinning solution is formed, the spinning solution is placed in a spinning solution storage tank after standing and defoaming, and the aperture of a spinneret plate is 0.25 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 2: 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 the PEDOT (PSS) spinning solution at a constant speed, wherein the advancing speed is 10 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, and collecting the fibers by a polytetrafluoroethylene roller. The stress-strain curve of the PEDOT PSS fiber spun by the comparative example is shown in FIG. 6, the tensile elongation is 11%, and the electrical conductivity is 0.06S/cm, as shown in FIG. 9.
Comparative example 3
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 20 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 uniform dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the aperture of a spinneret plate is 0.33 mm;
then, a coagulation bath was prepared: the coagulation bath in the comparative example was a mixed solution consisting of ethanol, water and KCl, the volume ratio of ethanol to water being 5: 1; the KCl is added at a concentration of 0.1 mol/L. Firstly, dissolving KCl in water, adding ethanol, and fully stirring for later use;
and finally, wet spinning: and extruding the PEDOT (PSS) spinning solution at a constant speed, wherein the advancing 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, and collecting the fibers by a polytetrafluoroethylene roller. PSS fiber spun from this comparative example showed a stress-strain curve as shown in FIG. 7, a tensile elongation of 6.6%, and an electrical conductivity of 0.08S/cm as shown in FIG. 9.
Comparative example 4
Firstly, preparing PEDOT (Poly ethylene terephthalate) (PSS) spinning solution: concentrating the aqueous dispersion of PEDOT (PSS) to 20 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 uniform dispersed spinning solution, standing for defoaming, and then placing into a spinning solution storage tank, wherein the aperture 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 composed of ethanol, water and LiCl, the volume ratio of ethanol to water being 1: 0; the LiCl was added at a concentration of 0.1 mol/L. Firstly, dissolving LiCl in water, then adding ethanol and fully stirring for later use;
and finally, wet spinning: and extruding the PEDOT (PSS) spinning solution at a constant speed, wherein the advancing 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, and collecting the fibers by a polytetrafluoroethylene roller. The stress-strain curve of the PEDOT PSS fiber spun by the comparative example is shown in FIG. 8, the tensile elongation is 14.3%, and the electrical conductivity is 1.67S/cm, as shown in FIG. 9.

Claims (6)

1. A spinning method of PEDOT PSS conductive fibers with high elongation is characterized by comprising the following steps:
the first step is as follows: preparing PEDOT, namely PSS spinning solution;
the second step is that: enabling the spinning solution to enter a mixed coagulating bath of ethanol and water through a wet spinning spinneret for coagulating and forming, wherein LiCl is added into the mixed coagulating bath of the ethanol and the water, and the addition concentration is 0.1-0.5 mol/L; and drawing, drying and cooling the solidified and formed fiber to prepare the PEDOT (PSS) conductive fiber with high conductivity and high elongation.
2. The spinning method of the PEDOT PSS conductive fiber with high elongation rate according to claim 1, wherein in the first step, the PEDOT PSS spinning solution is at normal temperature, the PEDOT PSS water dispersion solution is vibrated for 5-30 min by an ultrasonic oscillator, and after being uniformly mixed, the PEDOT PSS water dispersion solution is kept stand and defoamed to obtain the uniform spinning solution.
3. The spinning method of the high-elongation PEDOT PSS conductive fiber according to claim 2, wherein the dispersion concentration of PEDOT PSS is 15-25 mg/mL; the working frequency of the ultrasonic oscillator is 30-60 KHz.
4. PSS conductive fiber spinning process according to claim 1, characterized in that in the second step, in a mixed coagulation bath, the volume ratio of ethanol to water is: (2-5): 1.
5. PSS conductive fiber spinning process of PEDOT with high elongation according to claim 1, characterized in that in the second step, the spinneret hole diameter of the jet spinning solution is 0.13-0.51 mm.
6. PSS conductive fiber spinning method of PEDOT with high elongation according to claim 1, characterized in that in the second step, the fiber drawing method after coagulation forming in coagulation bath is: and fishing out the fiber when the fiber reaches the bottom of the coagulating bath, drying the fiber, and winding the fiber to the periphery of a polytetrafluoroethylene rod or a roller.
CN202010777076.0A 2020-08-05 2020-08-05 Spinning method of PEDOT (polyethylene glycol terephthalate): PSS (Poly styrene) conductive fiber with high elongation Active CN111793853B (en)

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CN114108132B (en) * 2021-11-17 2024-05-10 江苏大学 Preparation method of high-strength high-conductivity PEDOT fiber
CN115110168B (en) * 2022-06-24 2024-04-12 苏州大学 Manufacturing method of polytetrafluoroethylene fiber with high quality density uniformity

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