CN103981720A - Polyaniline (PANI)-modified aramid fiber (ARF) composite conductive fiber and preparation method thereof - Google Patents
Polyaniline (PANI)-modified aramid fiber (ARF) composite conductive fiber and preparation method thereof Download PDFInfo
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- CN103981720A CN103981720A CN201410241476.4A CN201410241476A CN103981720A CN 103981720 A CN103981720 A CN 103981720A CN 201410241476 A CN201410241476 A CN 201410241476A CN 103981720 A CN103981720 A CN 103981720A
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- 229920006231 aramid fiber Polymers 0.000 title claims abstract description 61
- 239000000835 fiber Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920000767 polyaniline Polymers 0.000 title abstract description 18
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 27
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 18
- 230000007935 neutral effect Effects 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 239000006227 byproduct Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000004760 aramid Substances 0.000 claims description 6
- 229920003235 aromatic polyamide Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 239000004519 grease Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 125000003700 epoxy group Chemical group 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 3
- 238000005727 Friedel-Crafts reaction Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005530 etching Methods 0.000 abstract description 2
- 238000010559 graft polymerization reaction Methods 0.000 abstract 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000004577 thatch Substances 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a polyaniline (PANI)-modified aramid fiber (ARF) composite conductive fiber and a preparation method thereof. The ARF has a smooth surface and relatively strong chemical inertness and is difficult in adsorbing aniline monomers to obtain the composite conductive fiber. The preparation method is characterized by using the ARF as a base material, etching the surface of the ARF by using a sodium hydroxide solution to generate obvious pit defects on the surface of the ARF, modifying the surface of the ARF by using epoxy chloropropane based on the Friedel-Crafts reaction, introducing an epoxy group with relatively high reaction activity to the benzene ring of a molecular main chain of the ARF and carrying out graft polymerization on aniline on the ARF by using the epoxy group as an active point, thus preparing the composite conductive fiber. The composite conductive fiber and the preparation method have the advantages that the surface of the ARF is modified, thus reducing the chemical inertness of the surface of the ARF; the prepared composite conductive fiber has low resistivity and excellent conductivity.
Description
Technical field
the present invention relates to a kind of conductive fiber, be specifically related to a kind of polyaniline-modifying aramid fiber composite conducting fiber and preparation method thereof.
Background technology
In numerous conducting polymers, polyaniline (PANI) has higher conductance, and raw material is cheap, stable performance, and synthetic method is simple, the clear and doping level of Doping Mechanism can be controlled, thereby becomes current one of the Structural electric Polymer material that obtains commercial Application that is hopeful most.But because the interaction of molecule chain rigidity and interchain polarity makes its dissolubility extremely low, be dissolved in hardly any organic solvent, brought difficulty to film forming and the processing of doped polyaniline, seriously hindered its large-scale promotion application in every field.Therefore the processing characteristics of improving polyaniline is to promote the practical key problem in technology of polyaniline.Existing research shows, can overcome the shortcoming of its poor in processability by polyaniline composite modification technology, obtains and has polyfunctional composite, expands its Application Areas.
Aramid fiber (Aramid fiber, ARF), is a kind of novel high-tech synthetic fiber, has superhigh intensity, high-modulus, high temperature resistant, acid-fast alkali-proof and the premium properties such as lightweight, is the novel special purpose synthetic fiber of a class.Because ARF has the advantages such as superhigh intensity, high-modulus, high temperature resistant and acid-fast alkali-proof, being applied to prepare composite fibre not only can make fiber have good electric conductivity, the mechanical property that can also keep preferably matrix fiber, compound by PANI and ARF, preparation PANI/ARF composite conducting fiber, be to prepare at present PANI conductive fiber one of the most promising method, it makes the extensive use of PANI material become possibility.But the surface smoothing of ARF and have stronger chemical inertness, the active basic point that is difficult to find on ARF surface reaction, therefore prepares PANI/ARF composite conducting fiber, need to carry out surface modification treatment to improve its surface reaction activity to ARF.
Summary of the invention
The object of this invention is to provide a kind of polyaniline-modifying aramid fiber composite conducting fiber and preparation method thereof, aramid fiber is carried out to surface modification, reduce the chemical inertness of aramid fiber surface, be beneficial to the compound of PANI and ARF.
The technical solution adopted in the present invention is:
The preparation method of polyaniline-modifying aramid fiber composite conducting fiber, is characterized in that:
By following steps, realized:
Step 1: the grease that cleans aramid fiber surface, get the undressed aramid fiber of 2 g, be placed in 100 mL acetone, ultrasonic 30 min, then with distilled water, clean, and to be placed in mass fraction be 5% sodium dodecyl sulfate aqueous solution, again ultrasonic 30 min, finally with distilled water, cleaning, drying are standby repeatedly;
It is 1% sodium hydroxide solution that the aramid fiber cleaning is put into mass fraction, stirs 2 h under reflux temperature, is washed till filtrate is afterwards neutral with distilled water, dries, and prepares the ARF of alkali treatment, is designated as SH-ARF;
Step 2: add 1.5 g SH-ARF fibers in there-necked flask, add 150 mL epoxychloropropane, start to stir, system is warming up to 95
oc, stirs 3 h, between this stage of reaction, repeatedly adds on a small quantity 1 g anhydrous Aluminum chloride in batches, by product suction filtration, clean with distilled water flushing after fully reacting, afterwards 60
osodium hydroxide solution with 5% under C soaks 1 h, is washed till filtrate and is neutral, and be dried after being disposed with distilled water, prepares epoxychloropropane modified ARF fiber, is designated as ECP-ARF;
Step 3: 0.1-1gECP-ARF is soaked in to 15-90 min in 1-5 mL aniline, and then join 90 mL molal volume concentration is in the hydrochloric acid solution of 0.5-3 mol/L, at 0-35 simultaneously
ounder C condition, drip ammonium persulfate solution 20 mL, the mol ratio of controlling ammonium persulfate and aniline monomer is (0.5:1)-(2.5:1), cause aniline monomer at ECP-ARF surface aggregate, react after 9 h, by product suction filtration, with distilled water, be washed till filtrate and be neutral, dry under room temperature, be prepared into polyaniline-modifying aramid fiber composite conducting fiber.
Described aramid fiber is para-aramid fiber or meta-aramid fibers.
As described in polyaniline-modifying aramid fiber composite conducting fiber of making of the preparation method of polyaniline-modifying aramid fiber composite conducting fiber.
The present invention has the following advantages:
The present invention carries out surface modification with epoxychloropropane to aramid fiber, introduces the epoxide group that reactivity is larger on the molecular backbone of aramid fiber, to reduce the chemical inertness on ARF surface.Meanwhile, aniline can be as active site, glycerol polymerization on ARF, thus being more conducive to prepare the PANI/ARF composite conducting fiber that resistivity is lower, resistivity is 2.0 * 10
5Ω m-7.5 * 10
5within the scope of Ω m.
The specific embodiment
Below in conjunction with the specific embodiment, the present invention will be described in detail.
The present invention be take ARF as base material, uses sodium hydroxide solution to carry out etching to it, makes ARF surface produce obvious indenture defect.Then, based on Fu Lide-Kerafyrm thatch reaction (Friedel-Crafts reaction, parent's electricity on phenyl ring replaces), use epoxychloropropane (ECP) to carry out surface modification to its ARF, on phenyl ring, introduce the epoxide group that reactivity is larger, make the aniline can be as active site, glycerol polymerization on ARF, thereby the PANI/ECP-ARF composite conducting fiber of preparation excellent electric conductivity.Specifically by following steps, realized:
Step 1: the grease that cleans aramid fiber surface, get the undressed aramid fiber of 2 g (para-aramid fiber or meta-aramid fibers), be placed in 100 mL acetone, ultrasonic 30 min, then with distilled water, clean, and to be placed in mass fraction be 5% sodium dodecyl sulfate aqueous solution, again ultrasonic 30 min, finally with distilled water, cleaning, drying are standby repeatedly;
It is 1% sodium hydroxide solution that the aramid fiber cleaning is put into mass fraction, stirs 2 h under reflux temperature, is washed till filtrate is afterwards neutral with distilled water, dries, and prepares the ARF of alkali treatment, is designated as SH-ARF;
Step 2: add 1.5 g SH-ARF fibers in there-necked flask, add 150 mL epoxychloropropane, start to stir, system is warming up to 95
oc, stirs 3 h, between this stage of reaction, repeatedly adds on a small quantity 1 g anhydrous Aluminum chloride in batches, by product suction filtration, clean with distilled water flushing after fully reacting, afterwards 60
osodium hydroxide solution with 5% under C soaks 1 h, is washed till filtrate and is neutral, and be dried after being disposed with distilled water, prepares epoxychloropropane modified ARF fiber, is designated as ECP-ARF;
Step 3: 0.1-1gECP-ARF is soaked in to 15-90 min in 1-5 mL aniline, and then join 90 mL molal volume concentration is in the hydrochloric acid solution of 0.5-3 mol/L, 0-35 simultaneously
ounder C condition, drip ammonium persulfate solution 20 mL, the mol ratio of controlling ammonium persulfate and aniline monomer is (0.5:1)-(2.5:1), cause aniline monomer at ECP-ARF surface aggregate, react after 9 h, by product suction filtration, with distilled water, be washed till filtrate and be neutral, dry under room temperature, be prepared into polyaniline-modifying aramid fiber composite conducting fiber.
Embodiment 1:
Step 1: the grease that cleans aramid fiber surface, get the undressed aramid fiber of 2 g (para-aramid fiber or meta-aramid fibers), be placed in 100 mL acetone, ultrasonic 30 min, then with distilled water, clean, and to be placed in mass fraction be 5% sodium dodecyl sulfate aqueous solution, again ultrasonic 30 min, finally with distilled water, cleaning, drying are standby repeatedly;
It is 1% sodium hydroxide solution that the aramid fiber cleaning is put into mass fraction, stirs 2 h under reflux temperature, is washed till filtrate is afterwards neutral with distilled water, dries, and prepares the ARF of alkali treatment, is designated as SH-ARF;
Step 2: add 1.5 g SH-ARF fibers in there-necked flask, add 150 mL epoxychloropropane, start to stir, system is warming up to 95
oc, stirs 3 h, between this stage of reaction, repeatedly adds on a small quantity 1 g anhydrous Aluminum chloride in batches, by product suction filtration, clean with distilled water flushing after fully reacting, afterwards 60
osodium hydroxide solution with 5% under C soaks 1 h, is washed till filtrate and is neutral, and be dried after being disposed with distilled water, prepares epoxychloropropane modified ARF fiber, is designated as ECP-ARF;
Step 3: 0.1gECP-ARF is soaked in to 15 min in 1 mL aniline, and then join 90 mL molal volume concentration is in the hydrochloric acid solution of 0.5 mol/L, 0 simultaneously
ounder C condition, drip ammonium persulfate solution 20 mL, the mol ratio of controlling ammonium persulfate and aniline monomer is 0.5:1, cause aniline monomer at ECP-ARF surface aggregate, after reaction 9 h, by product suction filtration, with distilled water, be washed till filtrate and be neutral, dry under room temperature, be prepared into polyaniline-modifying aramid fiber composite conducting fiber, recording its resistivity is 7.5 * 10
5Ω m.
Embodiment 2:
Step 1: the grease that cleans aramid fiber surface, get the undressed aramid fiber of 2 g (para-aramid fiber or meta-aramid fibers), be placed in 100 mL acetone, ultrasonic 30 min, then with distilled water, clean, and to be placed in mass fraction be 5% sodium dodecyl sulfate aqueous solution, again ultrasonic 30 min, finally with distilled water, cleaning, drying are standby repeatedly;
It is 1% sodium hydroxide solution that the aramid fiber cleaning is put into mass fraction, stirs 2 h under reflux temperature, is washed till filtrate is afterwards neutral with distilled water, dries, and prepares the ARF of alkali treatment, is designated as SH-ARF;
Step 2: add 1.5 g SH-ARF fibers in there-necked flask, add 150 mL epoxychloropropane, start to stir, system is warming up to 95
oc, stirs 3 h, between this stage of reaction, repeatedly adds on a small quantity 1 g anhydrous Aluminum chloride in batches, by product suction filtration, clean with distilled water flushing after fully reacting, afterwards 60
osodium hydroxide solution with 5% under C soaks 1 h, is washed till filtrate and is neutral, and be dried after being disposed with distilled water, prepares epoxychloropropane modified ARF fiber, is designated as ECP-ARF;
Step 3: 0.2gECP-ARF is soaked in to 30 min in 2 mL aniline, and then join 90 mL molal volume concentration is in the hydrochloric acid solution of 1 mol/L, 20 simultaneously
ounder C condition, drip ammonium persulfate solution 20 mL, the mol ratio of controlling ammonium persulfate and aniline monomer is 1:1, cause aniline monomer at ECP-ARF surface aggregate, after reaction 9 h, by product suction filtration, with distilled water, be washed till filtrate and be neutral, dry under room temperature, be prepared into polyaniline-modifying aramid fiber composite conducting fiber, recording its resistivity is 6.0 * 10
5Ω m.
Embodiment 3:
Step 1: the grease that cleans aramid fiber surface, get the undressed aramid fiber of 2 g (para-aramid fiber or meta-aramid fibers), be placed in 100 mL acetone, ultrasonic 30 min, then with distilled water, clean, and to be placed in mass fraction be 5% sodium dodecyl sulfate aqueous solution, again ultrasonic 30 min, finally with distilled water, cleaning, drying are standby repeatedly;
It is 1% sodium hydroxide solution that the aramid fiber cleaning is put into mass fraction, stirs 2 h under reflux temperature, is washed till filtrate is afterwards neutral with distilled water, dries, and prepares the ARF of alkali treatment, is designated as SH-ARF;
Step 2: add 1.5 g SH-ARF fibers in there-necked flask, add 150 mL epoxychloropropane, start to stir, system is warming up to 95
oc, stirs 3 h, between this stage of reaction, repeatedly adds on a small quantity 1 g anhydrous Aluminum chloride in batches, by product suction filtration, clean with distilled water flushing after fully reacting, afterwards 60
osodium hydroxide solution with 5% under C soaks 1 h, is washed till filtrate and is neutral, and be dried after being disposed with distilled water, prepares epoxychloropropane modified ARF fiber, is designated as ECP-ARF;
Step 3: 1gECP-ARF is soaked in to 90 min in 5 mL aniline, and then join 90 mL molal volume concentration is in the hydrochloric acid solution of 3 mol/L, 35 simultaneously
ounder C condition, drip ammonium persulfate solution 20 mL, the mol ratio of controlling ammonium persulfate and aniline monomer is 2.5:1, cause aniline monomer at ECP-ARF surface aggregate, after reaction 9 h, by product suction filtration, with distilled water, be washed till filtrate and be neutral, dry under room temperature, be prepared into polyaniline-modifying aramid fiber composite conducting fiber, recording its resistivity is 2.0 * 10
5Ω m.
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading description of the present invention, is claim of the present invention and contains.
Claims (3)
1. the preparation method of polyaniline-modifying aramid fiber composite conducting fiber, is characterized in that:
By following steps, realized:
Step 1: the grease that cleans aramid fiber surface, get the undressed aramid fiber of 2 g, be placed in 100 mL acetone, ultrasonic 30 min, then with distilled water, clean, and to be placed in mass fraction be 5% sodium dodecyl sulfate aqueous solution, again ultrasonic 30 min, finally with distilled water, cleaning, drying are standby repeatedly;
It is 1% sodium hydroxide solution that the aramid fiber cleaning is put into mass fraction, stirs 2 h under reflux temperature, is washed till filtrate is afterwards neutral with distilled water, dries, and prepares the ARF of alkali treatment, is designated as SH-ARF;
Step 2: add 1.5 g SH-ARF fibers in there-necked flask, add 150 mL epoxychloropropane, start to stir, system is warming up to 95
oc, stirs 3 h, between this stage of reaction, repeatedly adds on a small quantity 1 g anhydrous Aluminum chloride in batches, by product suction filtration, clean with distilled water flushing after fully reacting, afterwards 60
osodium hydroxide solution with 5% under C soaks 1 h, is washed till filtrate and is neutral, and be dried after being disposed with distilled water, prepares epoxychloropropane modified ARF fiber, is designated as ECP-ARF;
Step 3: 0.1-1gECP-ARF is soaked in to 15-90 min in 1-5 mL aniline, and then join 90 mL molal volume concentration is in the hydrochloric acid solution of 0.5-3 mol/L, at 0-35 simultaneously
ounder C condition, drip ammonium persulfate solution 20 mL, the mol ratio of controlling ammonium persulfate and aniline monomer is (0.5:1)-(2.5:1), cause aniline monomer at ECP-ARF surface aggregate, react after 9 h, by product suction filtration, with distilled water, be washed till filtrate and be neutral, dry under room temperature, be prepared into polyaniline-modifying aramid fiber composite conducting fiber.
2. the preparation method of polyaniline-modifying aramid fiber composite conducting fiber according to claim 1, is characterized in that:
Described aramid fiber is para-aramid fiber or meta-aramid fibers.
3. polyaniline-modifying aramid fiber composite conducting fiber that the preparation method of polyaniline-modifying aramid fiber composite conducting fiber as claimed in claim 2 makes.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108193499A (en) * | 2017-12-20 | 2018-06-22 | 苏州禾川化学技术服务有限公司 | A kind of fiber metallizing treatment process |
| CN110628215A (en) * | 2019-10-08 | 2019-12-31 | 陕西科技大学 | Polyaniline/aramid nanofiber conductive composite film and preparation method thereof |
| CN110725124A (en) * | 2019-12-04 | 2020-01-24 | 中国科学院兰州化学物理研究所 | Interface enhancement method for para-aramid-polytetrafluoroethylene blended fiber fabric |
| CN110761077A (en) * | 2019-10-20 | 2020-02-07 | 南京理工大学 | Conductive polyaniline @ aramid nanofiber composite film material and preparation method thereof |
| CN111653433A (en) * | 2020-06-09 | 2020-09-11 | 陕西科技大学 | Polyaniline/silver nanowire cotton fiber capacitor electrode material and preparation method thereof |
| CN115679705A (en) * | 2021-07-21 | 2023-02-03 | 北京服装学院 | Conductive fiber and conductive fabric as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110761077A (en) * | 2019-10-20 | 2020-02-07 | 南京理工大学 | Conductive polyaniline @ aramid nanofiber composite film material and preparation method thereof |
| CN110761077B (en) * | 2019-10-20 | 2022-05-13 | 南京理工大学 | Conductive polyaniline @ aramid nanofiber composite film material and preparation method thereof |
| CN110725124A (en) * | 2019-12-04 | 2020-01-24 | 中国科学院兰州化学物理研究所 | Interface enhancement method for para-aramid-polytetrafluoroethylene blended fiber fabric |
| CN111653433A (en) * | 2020-06-09 | 2020-09-11 | 陕西科技大学 | Polyaniline/silver nanowire cotton fiber capacitor electrode material and preparation method thereof |
| CN115679705A (en) * | 2021-07-21 | 2023-02-03 | 北京服装学院 | Conductive fiber and conductive fabric as well as preparation method and application thereof |
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| CN103981720B (en) | 2016-04-20 |
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