CN105839228A - Method for preparing polyacrylonitrile-based conductive fiber material - Google Patents
Method for preparing polyacrylonitrile-based conductive fiber material Download PDFInfo
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- CN105839228A CN105839228A CN201610382926.0A CN201610382926A CN105839228A CN 105839228 A CN105839228 A CN 105839228A CN 201610382926 A CN201610382926 A CN 201610382926A CN 105839228 A CN105839228 A CN 105839228A
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention provides a polyacrylonitrile-based conductive fiber material and a method for preparing the same. The polyacrylonitrile-based conductive fiber material and the method have the advantages that polyacrylonitrile is used as a template, anionic surfactants are used as emulsifiers and dopants, conductive polymers are directly polymerized on the surfaces of polyacrylonitrile fibers by the aid of the template polymerization method, dense coating layers can be formed on the surfaces of the polyacrylonitrile fibers by the conductive polymers, and accordingly the polyacrylonitrile-based conductive fiber material with conductivity properties can be prepared; the polyacrylonitrile has certain conductivity, and accordingly conductive or antistatic effects can be realized by the polyacrylonitrile; polyaniline coated polyacrylonitrile fiber films are subjected to high-temperature carbonization treatment in order to further expand the application range, and a novel carbon fiber material can be obtained; the novel carbon fiber material is excellent in supercapacitor performance and can be used as an electrode material for supercapacitors.
Description
Technical field
The present invention relates to a kind of conductive fiber and preparation method thereof, be specifically related to the system of a kind of polyacrylonitrile-radical conductive fiber material
Preparation Method.
Background technology
Intrinsic conducting polymer is owing to having special structure and excellent physicochemical characteristics so that it is electrochromic display device,
Rechargeable battery and fuel cell, the electrode material of ultracapacitor, electromagnetic shielding material, microwave absorption stealth material, electroluminescent
Optical device positive pole decorative material, sensor, transparent conducting coating, conductive fiber, polymer photovoltaic cell material and heavy metal from
The aspects such as sub-absorption have extensive and tempting application prospect.Intrinsic conducting polymer is often the polymer of a kind of indissoluble infusibility,
There is certain difficulty in processing, limit its application.Therefore, Recent study person are matrix with different fibers and fabric
Prepare conducting polymer conductive fiber composite material.Utilize matrix polymerization method that conducting polymer is deposited on fiber surface, keeping
Electric conductivity is obtained while matrix some strength.Such as, Zhang Huiqin etc., " a kind of polyacrylonitrile/pocompounde compounde micro-nano is led
The preparation method of electricity fiber " (Chinese patent CN103255634A) be prepared for polyacrylonitrile micro nanometer fiber by electrostatic spinning,
Then by template at fiber surface parcel one strata aniline in situ, conductive polymer micro-nano rice composite fibre is obtained.Hui Zhou
Deng, by template, hydrochloric acid acid doped polyaniline being aggregated in method of electrostatic spinning and prepare polytetrafluoroethylfiber fiber film surface, preparation is poly-
Aniline/polytetrafluoroethylcomposite composite film, this fibrous membrane has preferable electric conductivity, has the property of excellence at absorbing heavy metal ions
Can (Hui Zhou, Zhiquan Shi, Yun Lu.Conducting polyaniline/poly (tetrafluoroethylene) composite
Films with tunable surface morphology and hydrophilicity [J] .Synthetic Metals, 2010,160:
1925-1930.).Nanofiber has that specific surface area is big, porosity high, and micro/nano fibrous membrane material has small size effect
Should, skin effect etc..The preparation method of common nanofiber has method of electrostatic spinning, centrifugal spinning, template drawing-off etc..Mesh
Before, solution jet spinning method (Zhuan Xupin, " preparation method of a kind of polymeric nano-micro fiber non-woven fabric " (Chinese patent
CN102071542A)) being paid close attention to as a kind of novel method preparing nanofiber, the method has efficiency height, energy consumption
The advantages such as low, technique is simple.That conducting polymer is deposited on is prepared by solution jet spinning method herein by matrix polymerization method poly-third
Alkene nitrile fibrous membrane surface, has prepared and has had stable, the composite cellulosic membrane of lasting electric conductivity, and this composite may be used for conduction
The aspects such as textile, solaode, energy storage material, sensor and water process.
In order to expand the range of application of prepared composite cellulosic membrane further, herein it is carried out carbonization treatment to be applied to surpass
Level capacitor aspect.Ultracapacitor, as a kind of novel electrochemical energy storage device, has that electrode material is abundant, discharge and recharge speed
The features such as degree is fast, environmental friendliness, by whole world scientist and the extensive concern of government department.Ultracapacitor can be applied
Some need in the product of quick charge, such as electric motor car, pocket lamp etc., and in addition it can also store as static random
The back-up source that the Weak current such as device, data transmission system is powered.Along with widening of its application, the market demand is also progressively
Improving, the most how preparing inexpensive electrode material becomes the key of research.Fiber-like material with carbon element is widely used in super
Capacitor electrode material, the present invention is a kind of new by polyaniline/polyacrylonitrile core-skin composite fiber film high-temp. carbonization treatment being obtained
Carbon fibre material, this composite can be as electrode material for super capacitor.
Summary of the invention
The invention provides a kind of conducting polypropylene nitrile fibrous material and preparation method thereof, this conductive fiber material spins with solution injection
Polyacrylonitrile fibre membrane prepared by silk method is template, and anion surfactant is not only emulsifying agent but also be adulterant, uses template to gather
The method closed, prepares conducting polypropylene nitrile fibrous material.This makes polyacrylonitrile fibre have certain electrical conductivity, has simultaneously
The performance of Adsorption of Heavy Metal Ions, expands the range of application of polyacrylonitrile.Further it is carried out high temperature cabonization process, prepare
A kind of material with carbon element with preferable super capacitor performance, can use as electrode material for super capacitor.
1. the present invention prepares specifically comprising the following steps that of a kind of conducting polypropylene nitrile fibrous material
(1) preparation of spinning solution: be dissolved in solvent by polyacrylonitrile, forming mass concentration is 4～30% homogeneous spinning
Solution；
(2) polyacrylonitrile solution that step (1) is obtained, use solution jet spinning method prepare polyacrylonitrile micro-/receive
Rice fibrous membrane；
(3) a certain amount of demulsifier is mixed homogeneously by a certain percentage with deionized water, add a certain amount of anion surfactant and join
Become 0.05～1mol/L mixed solution；
(4) by the nano fibrous membrane of system in step (2), take in the mixed solution of a certain amount of addition step (3) and be sufficiently impregnated with
5～30min.It is subsequently adding monomer, monomer concentration 0.5～2mol/L, under room temperature, stirs 10～60min；
(5) adding oxidant in step (4) system, oxidant concentration is 0.3～4mol/L, changes at 0～30 DEG C
Learning oxidation polymerization, stir 6～8h, mixing speed controls 1～1000rpm, then stands 10～24h.After reaction terminates, will
Reactant filters, and it is colourless for fully washing to filtrate with organic solvent, deionized water successively, dries 10～48h for 50～120 DEG C,
Obtain conducting polypropylene nitrile fibrous material；
(6) pre-oxidation treatment: conducting polypropylene nitrile fibrous material step (5) obtained pre-oxidizes in air atmosphere
Obtaining pre-oxidized fibers, Pre oxidation is 160～300 DEG C, and preoxidation time is 2～3h；
(7) carbonization treatment: pre-oxidized fibers step (6) obtained carries out carbonization treatment in nitrogen or argon atmosphere and obtains
Carbon fiber, carburizing temperature is 600～1300 DEG C, and carbonization time is 0.5～3h.
Wherein in step (1), polyacrylonitrile is polyacrylonitrile homopolymer or copolymer, and viscosity-average molecular weight is 8～300,000, wherein
Acrylonitrile segment accounts for more than 85%, remaining be acrylic acid methyl ester., acrylic acid, acrylamide, itaconic acid, Sodium styrene sulfonate or
Sodium allylsulfonate.
3. described in step (1), solvent is in DMF, N,N-dimethylacetamide, dimethyl sulfoxide
Planting or two kinds and above mixture, solution temperature scope is that room temperature is to 100 DEG C.
4. during described in step (2), solution jet spinning method prepares polyacrylonitrile micro/nano-fibre felt, impact fibre
The viscosity 1000-10000mPa s that technological parameter is high polymeric solution of the diameter of dimension, fltting speed 0.5-50ml/h, spinneret orifice
A diameter of 0.05-1.25mm, air-flow slit is 0.02-0.75mm, and air inlet stream amount is 300-1200m3/ h, aerofluxus implication
Flow is 1600-3200m3/ h, size 0.01-0.8MPa of spinning air pressure, temperature 20-380 DEG C of air-flow, receiving range 0.4-10
The factors such as m.
5. demulsifier described in step (3) be in methanol, ethanol, acetone and butanone one or both and more than.With go from
The ratio of sub-water is 1: 1～5.
6. described in step (3), anion surfactant is sodium lauryl sulphate, sodium hexadecyl sulfate, dodecyl
Benzenesulfonic acid and salt thereof, cetyl benzenesulfonic acid and salt thereof, ethyoxyl alkyl sodium sulfate, ethyoxyl alkyl ammonium sulfate, polyacrylic acid
And salt, alkylpolyoxyethylene sodium sulfate, sodium soap, alkylpolyoxyethylene carboxylic acid sodium, di-2-ethylhexylphosphine oxide naphthalene
In sodium sulfonate one or both and more than.Anion surfactant is both as emulsifying agent, again as the adulterant of polyaniline.
Solution concentration is 0.05～1mol/L.
7. described in step (4), monomer is pyrroles, aniline, thiophene, in 3,4-ethylene dioxythiophene one or both and with
On.Monomer concentration is 0.5～2mol/L.
8. described in step (5), oxidant is ferric chloride, hydrogen peroxide, Ammonium persulfate., aluminum chloride, potassium permanganate, weight
Neutral potassium chromate, potassium iodate, in manganese dioxide one or both and more than.Oxidant concentration is 0.1～4mol/L.
9. preparation method as claimed in claim 1, described in prepare polyaniline/polyacrylonitrile composite conductive fibre and can apply
In solaode, energy storage material, sensor and the aspect such as heavy metal ion adsorbed.
10. preparation method as claimed in claim 1, the application of described silicon carbide/polypropylene itrile group conductive fiber is lithium ion secondary
The fields such as battery anode material, electrical double layer capacitor electrodes, high-efficiency adsorbent, Heat Conduction Material, field electron emission materials.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 solution spurt method prepares polyacrylonitrile fibre membrane figure (scanning electron micrographs).
Fig. 2 is that embodiment 1 solution spurt method prepares polyacrylonitrile fibre membrane figure.
Fig. 3 is embodiment 1 polyaniline-coated conducting polypropylene nitrile fibrous membrane figure (scanning electron micrographs).
Fig. 4 is the polyaniline-coated conducting polypropylene nitrile fibrous membrane figure obtained by embodiment 1.
Fig. 5 is the composite cellulosic membrane figure after embodiment 1 high temperature cabonization.(scanning electron micrographs).
Detailed description of the invention
Below by way of specific embodiment for further illustrating the method that the present invention describes, it is not intended that the present invention is limited to
These embodiments.
Embodiment 1:
A kind of polyacrylonitrile-radical conductive fiber material preparation method, comprises the steps:
(1) preparation of spinning solution: the polyacrylonitrile of viscosity-average molecular weight 90,000 is dissolved in N with the ratio of mass fraction 12%,
In dinethylformamide, stirring, to mix homogeneously, makes spinning liquid；
(2) solution jet spinning method prepares polyacrylonitrile fibre material: through dosing pump, spinning solution is fed to spinneret die,
Spinning solution is made to be extruded into spinning solution thread from the spinneret orifice of spinneret die；Blow to extrusion with high velocity jet air-flow spin simultaneously
Silk solution thread, high velocity air stretching solution thread also promotes that solvent volatilization is allowed to form polyacrylonitrile micro/nano-fibre.Relevant work
Skill parameter is: the apparent viscosity of solution is 8058mPa s, and gas flow temperature is 80 DEG C, and fltting speed is 5ml/h, and spinneret orifice is straight
Footpath is 0.3mm, and air-flow slit is 0.2mm, air inlet stream amount 700m3/ h, throughput 1800m of air vent3/ h, spins
Silk air pressure is 0.15MPa, and receiving range is 80cm；
(3) a certain amount of ethanol is mixed homogeneously with deionized water volume ratio 1: 5, add a certain amount of DBSA and be made into
0.3mol/L mixed solution；
(4) by step (2) system polyacrylonitrile fibre membrane, take in the mixed solution of a certain amount of addition step (3) and fill
Sub-dip stain 10min.It is subsequently adding aniline monomer, monomer concentration 0.5mol/L, under room temperature, stirs 30min；
(5) in step (4) system, addition Ammonium persulfate. is as oxidant, and oxidant concentration is 0.5mol/L, at 0 DEG C
Under carry out chemical oxidising polymerisation, stir 6h, mixing speed controls at 800rpm, then stands 12h.After reaction terminates, will
Reactant filters, and it is colourless for fully washing to filtrate with ethanol, deionized water successively, dries 24h, obtains conducting electricity poly-third for 50 DEG C
Alkene nitrile fibrous material；
(6) pre-oxidation treatment: conducting polypropylene nitrile fibrous material step (5) obtained pre-oxidizes in air atmosphere
Obtaining pre-oxidized fibers, Pre oxidation is 280 DEG C, and preoxidation time is 2h；
(7) carbonization treatment: pre-oxidized fibers step (6) obtained carries out carbonization treatment in nitrogen atmosphere and obtains carbon fiber,
5 DEG C/min of heating rate, carburizing temperature is 700 DEG C, and carbonization time is 2h.
Conducting polypropylene nitrile fibrous material obtained by preparation, Fig. 1 is polyacrylonitrile fibre prepared by solution spurt method, and Fig. 3 is poly-
The composite fibre scanning electron microscope (SEM) photograph that aniline cladding polyacrylonitrile fibre material obtains, polyaniline is in fiber surface shape as seen from the figure
Become fine and close clad.Conductivity is up to 1.24x10-2S/cm.Fig. 5 is sweeping after polyaniline/polyacrylonitrile composite fiber high temperature cabonization
Retouch Electronic Speculum figure.
Embodiment 2:
As different from Example 1, step (4) is subsequently adding pyrrole monomer to the present embodiment, monomer concentration 0.5mol/L, its
It is same as in Example 1.
Embodiment 3:
As different from Example 1, step (4) is subsequently adding thiophene monomer to the present embodiment, monomer concentration 0.5mol/L, its
It is same as in Example 1.
Embodiment 4:
A kind of conducting polypropylene nitrile fibrous material preparation method, comprises the steps:
(1) preparation of spinning solution: the polyacrylonitrile of viscosity-average molecular weight 90,000 is dissolved in N with the ratio of mass fraction 12%,
In dinethylformamide, stirring, to mix homogeneously, makes spinning liquid；
(2) solution jet spinning method prepares polyacrylonitrile fibre material: through dosing pump, spinning solution is fed to spinneret die,
Spinning solution is made to be extruded into spinning solution thread from the spinneret orifice of spinneret die；Blow to extrusion with high velocity jet air-flow spin simultaneously
Silk solution thread, high velocity air stretching solution thread also promotes that solvent volatilization is allowed to form polyacrylonitrile micro/nano-fibre.Related process
Parameter is: the apparent viscosity of solution is 8058mPa s, and gas flow temperature is 80 DEG C, and fltting speed is 5ml/h, orifice diameter
For 0.3mm, air-flow slit is 0.2mm, air inlet stream amount 700m3/ h, throughput 1800m of air vent3/ h, spinning
Air pressure is 0.15MPa, and receiving range is 80cm；
(3) a certain amount of ethanol is mixed homogeneously with deionized water volume ratio 2: 5, add a certain amount of DBSA and be made into
0.3mol/L mixed solution；
(4) by the polyacrylonitrile fibre membrane of system in step (2), take in the mixed solution of a certain amount of addition step (3) abundant
Dipping 10min.It is subsequently adding aniline monomer, monomer concentration 0.5mol/L, under room temperature, stirs 30min；
(5) in step (4) system, addition Ammonium persulfate. is as oxidant, and oxidant concentration is 0.5mol/L, at 0 DEG C
Under carry out chemical oxidising polymerisation, stir 6h, mixing speed controls at 800rpm, then stands 12h.After reaction terminates, will
Reactant filters, and it is colourless for fully washing to filtrate with ethanol, deionized water successively, dries 24h, obtains conducting electricity poly-third for 50 DEG C
Alkene nitrile fibrous material；
(6) pre-oxidation treatment: conducting polypropylene nitrile fibrous material step (5) obtained pre-oxidizes in air atmosphere
Obtaining pre-oxidized fibers, Pre oxidation is 280 DEG C, and preoxidation time is 2h；
(7) carbonization treatment: pre-oxidized fibers step (6) obtained carries out carbonization treatment in nitrogen atmosphere and obtains carbon fiber,
5 DEG C/min of heating rate, carburizing temperature is 800 DEG C, and carbonization time is 2h.
Claims (10)
1. a preparation method for polyacrylonitrile-radical conductive fiber material, it comprises the steps:
(1) preparation of spinning solution: be dissolved in solvent by polyacrylonitrile, forming mass concentration is 4～30% homogeneous spinning
Solution.
(2) polyacrylonitrile solution that step (1) is obtained, use solution jet spinning method prepare polyacrylonitrile micro-/
Nano fibrous membrane.
(3) a certain amount of demulsifier is mixed homogeneously by a certain percentage with deionized water, add a certain amount of anion surfactant
It is made into 0.05～1mol/L mixed solution.
(4) by the nano fibrous membrane of system in step (2), take in the mixed solution of a certain amount of addition step (3) and be sufficiently impregnated with
5～30min.It is subsequently adding monomer, monomer concentration 0.5～2mol/L, under room temperature, stirs 10～60min.
(5) adding oxidant in step (4) system, oxidant concentration is 0.3～4mol/L, changes at 0～30 DEG C
Learning oxidation polymerization, stir 6～8h, mixing speed controls 1～1000rpm, then stands 10～24h.After reaction terminates, will
Reactant filters, and it is colourless for fully washing to filtrate with organic solvent, deionized water successively, dries 10～48h for 50～120 DEG C,
Obtain conducting polypropylene nitrile fibrous material.
(6) pre-oxidation treatment: conducting polypropylene nitrile fibrous material step (5) obtained pre-oxidizes in air atmosphere
Obtaining pre-oxidized fibers, Pre oxidation is 160～300 DEG C, and preoxidation time is 2～3h.
(7) carbonization treatment:: pre-oxidized fibers step (6) obtained carries out carbonization treatment in nitrogen or argon atmosphere and obtains
To carbon fiber, carburizing temperature is 600～1300 DEG C, and carbonization time is 0.5～3h.
2. preparation method as claimed in claim 1, in step (1), polyacrylonitrile is polyacrylonitrile homopolymer or copolymer,
Viscosity-average molecular weight is 8～300,000, and wherein acrylonitrile segment accounts for more than 85%, and remaining is acrylic acid methyl ester., acrylic acid, acryloyl
Amine, itaconic acid, Sodium styrene sulfonate or sodium allylsulfonate.
3. preparation method as claimed in claim 1, described in step (1), solvent is DMF, N, N-
One or both and above mixture in dimethyl acetylamide, dimethyl sulfoxide, solution temperature scope is that room temperature is to 100 DEG C.
4. preparation method as claimed in claim 1, described solution jet spinning method prepares polyacrylonitrile micro/nano-fibre
During felt, affect the viscosity 1000-10000mPa s that technological parameter is high polymeric solution of the diameter of fiber, fltting speed
0.5-50ml/h, orifice diameter is 0.05-1.25mm, and air-flow slit is 0.02-0.75mm, and air inlet stream amount is 300-1200
m3/ h, air vent throughput is 1600-3200m3/ h, size 0.01-0.8MPa of spinning air pressure, temperature 20-380 DEG C of air-flow,
The factors such as receiving range 0.4-10m.
5. preparation method as claimed in claim 1, described in step (3), demulsifier is in methanol, ethanol, acetone and butanone
One or more.It is 1: 1～5 with the ratio of deionized water.
6. preparation method as claimed in claim 1, described in step (3), anion surfactant is sodium lauryl sulphate,
Sodium hexadecyl sulfate, DBSA and salt thereof, cetyl benzenesulfonic acid and salt thereof, ethyoxyl alkyl sodium sulfate, second
Epoxide alkylsurfuric acid ammonium, polyacrylic acid and salt thereof, alkylpolyoxyethylene sodium sulfate, sodium soap, dodecyl polyoxy
Vinyl Ether carboxylic acid sodium, in sodium methylene bis-naphthalene sulfonate one or both and more than.Anion surfactant both as emulsifying agent,
Again as the adulterant of polyaniline.Solution concentration is 0.05～1mol/L.
7. preparation method as claimed in claim 1, described in step (4), monomer is pyrroles, aniline, thiophene, 3,4-ethylenes two
In oxygen thiophene one or both and more than.Monomer concentration is 0.5～2mol/L.
8. preparation method as claimed in claim 1, described in step (5), oxidant is ferric chloride, hydrogen peroxide, persulfuric acid
Ammonium, aluminum chloride, potassium permanganate, potassium dichromate, potassium iodate, in manganese dioxide one or both and more than.Oxidant is dense
Degree is 0.1～4mol/L.
9. preparation method as claimed in claim 1, described in prepare polyaniline/polyacrylonitrile composite conductive fibre and can apply
In solaode, energy storage material, sensor and the aspect such as heavy metal ion adsorbed.
10. preparation method as claimed in claim 1, the application of described silicon carbide/polypropylene itrile group conductive fiber is lithium ion secondary
The fields such as battery anode material, electrical double layer capacitor electrodes, high-efficiency adsorbent, Heat Conduction Material, field electron emission materials.
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| CN109267347A (en) * | 2018-09-27 | 2019-01-25 | 天津工业大学 | A kind of preparation method of polypyrrole/oxidization fiber felt flexible electromagnetic shielding material |
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| CN109913971A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of porous composite nano fiber and its preparation method and application |
| CN110184683A (en) * | 2019-05-07 | 2019-08-30 | 清华大学 | A kind of anisotropy stratiform carbon fiber-based aerogel material and preparation method thereof |
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| CN106868714A (en) * | 2017-02-20 | 2017-06-20 | 南通市中和化纤有限公司 | PAN micro nanometer fiber films are spun in heavy metal ion adsorbed liquid spray |
| US11286579B2 (en) * | 2017-03-27 | 2022-03-29 | Toray Industries, Inc. | Fiber production method and carbon fiber production method |
| CN109913971A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of porous composite nano fiber and its preparation method and application |
| CN108486690A (en) * | 2018-03-15 | 2018-09-04 | 上海应用技术大学 | A kind of nitrogen-doped carbon nano-fiber electrode material and preparation method thereof |
| CN109267347A (en) * | 2018-09-27 | 2019-01-25 | 天津工业大学 | A kind of preparation method of polypyrrole/oxidization fiber felt flexible electromagnetic shielding material |
| CN109763338A (en) * | 2018-12-29 | 2019-05-17 | 厦门大学 | A kind of polyacrylonitrile-based carbon fibre/polyaniline composite conductive fiber of core sheath structure and preparation method thereof |
| CN109763338B (en) * | 2018-12-29 | 2020-11-27 | 厦门大学 | Polyacrylonitrile-based carbon fiber/polyaniline composite conductive fiber with core-sheath structure and preparation method thereof |
| CN110184683A (en) * | 2019-05-07 | 2019-08-30 | 清华大学 | A kind of anisotropy stratiform carbon fiber-based aerogel material and preparation method thereof |
| CN114486861A (en) * | 2022-01-25 | 2022-05-13 | 东南大学 | Electrochemiluminescence molecular imprinting sensor and preparation method and application thereof |
| CN114486861B (en) * | 2022-01-25 | 2024-01-02 | 东南大学 | Electrochemiluminescence molecular imprinting sensor and preparation method and application thereof |
| CN115323784A (en) * | 2022-01-27 | 2022-11-11 | 青岛大学 | Polypyrrole conductive flexible fiber membrane material and preparation method thereof |
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