CN109537105A - A kind of porous hollow fiber conductive material and preparation method thereof - Google Patents
A kind of porous hollow fiber conductive material and preparation method thereof Download PDFInfo
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- CN109537105A CN109537105A CN201811325447.0A CN201811325447A CN109537105A CN 109537105 A CN109537105 A CN 109537105A CN 201811325447 A CN201811325447 A CN 201811325447A CN 109537105 A CN109537105 A CN 109537105A
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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
-
- 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
- D01D5/0007—Electro-spinning
-
- 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
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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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
- 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
- D01F1/08—Addition of substances to the spinning solution or to the melt for forming hollow 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
- 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
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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)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to functional fibre material field, a kind of porous hollow fiber conductive material and preparation method thereof is disclosed.Polyacrylonitrile is dissolved in organic solvent, pore former is added and is uniformly mixed, obtains cortex solution；Water-soluble high-molecular material is dissolved in deionized water, sandwich layer solution is obtained；By cortex solution and sandwich layer solution by electrostatic spinning, obtain with skin-core structure complex fiber material；By water-bath immersion and freeze-drying process, sandwich layer ingredient is removed, hollow fiber material is obtained；By hollow fiber material under an inert atmosphere by pre-oxidation and carbonization treatment, processing then is performed etching for pore former, obtains porous hollow fiber conductive material.Porous hollow fiber conductive material of the invention can guarantee the skin-core structure of conductive material, conduct electricity very well；And gathering for charge is reduced by skin-core structure and porous structure, charge density is reduced, the antistatic durability of material is improved.
Description
Technical field
The invention belongs to functional fibre material fields, and in particular to a kind of porous hollow fiber conductive material and its preparation side
Method.
Background technique
Carbon nanotube has great draw ratio, excellent mechanical strength and good conductive and heat-conductive ability, is a kind of
Ideal flexible conducting material；Graphene is by sp2The honeycomb structure of the carbon atom composition of hydridization, the thickness of single-layer graphene
Only 0.335nm, light transmittance are up to 97.7%, and Young's modulus reaches 1TPa, and it is most thin to be currently known intensity highest, thickness
Material, because of its splendid flexibility and electric conductivity, it is considered to be prepare the ideal material of flexible conducting material；Carbon nanotube and graphite
Alkene all has good flexible, outstanding conduction and thermal conductivity, excellent physics and chemical stability, and has structure and property
The features such as being readily susceptible to regulation, the application in flexible conducting material field has obtained extensive concern and substantive hair in recent years
Exhibition.
Electrostatic spinning is a kind of special fiber fabrication process, and polymer solution or melt carry out injection spinning in strong electrical field
Silk.Under electric field action, the drop at syringe needle can be become conical (i.e. " taylor cone ") from spherical shape, and be extended from conical tip
To fiber filaments.This mode can produce the polymer filaments of nanometer grade diameter.Electrostatic spinning technique is constructing a wiener
Rice structural material field has played very important effect, and it is more that structure has been successfully prepared out using electrostatic spinning technique
The nano-fiber material of sample.By different preparation methods, such as change nozzle structure, control experiment condition, reality can be obtained
The two-dimensional fiber film of the heart, hollow, nucleocapsid structure superfine fibre or spider reticulation structure；By designing different collection dresses
It sets, single fiber, fibre bundle, height-oriented fiber or random orientation tunica fibrosa etc. can be obtained.
Conductive fiber is commonly used in modern anti-static clothing fabric, the antistatic mechanism of conductive fiber is to make conduction
Corona discharge is generated between fiber.Corona discharge is a kind of discharge type mitigated very much, after electrostatic pressure reaches certain numerical value,
Generating nonarcing corona discharge makes static elimination.This phenomenon is commonly referred to be the conductive fiber in fabric, in electrostatic field
Under the action of, so that the air of surrounding is generated ionization and is formed negative ions, one of negative ions are with fabric institute with quiet
Opposite charge and neutralize, it is another then with environment or the earth neutralize, to eliminate electrostatic.
Existing conductive fiber mostly uses greatly post treatment method to process to obtain, and it is anti-mainly to carry out chemistry on general fibre surface
It answers, electroconductive polymer is made to be adsorbed on fiber surface, make the conductive energy of general fibre；Fiber is assigned using conductive compositions to lead
The performance of electricity, and used herein of conductive compositions, that is, conductive filler, and be mostly directly to coat carbon black or other gold in fiber surface
Belong to conductive paste, there are carbon black and metallic conduction slurry it is easy to fall off in fiber surface, being not easy to be uniformly distributed causes antistatic durability poor.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of porous
The preparation method of doughnut conductive material.
Another object of the present invention is to provide a kind of porous hollow fiber conduction materials being prepared by the above method
Material.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of porous hollow fiber conductive material, including following preparation step:
(1) preparation of cortex solution: polyacrylonitrile is dissolved in organic solvent, and pore former is then added and is stirred
It is even, obtain cortex solution；
(2) preparation of sandwich layer solution: water-soluble high-molecular material is dissolved in deionized water, obtains sandwich layer solution；
(3) cortex solution and sandwich layer solution are obtained by electrostatic spinning with skin-core structure complex fiber material；
(4) there will be skin-core structure complex fiber material by water-bath immersion and freeze-drying process, and remove skin-core structure
The sandwich layer ingredient of complex fiber material, obtains hollow fiber material；
(5) then hollow fiber material is carried out under an inert atmosphere by pre-oxidation and carbonization treatment for pore former
Etching processing obtains porous hollow fiber conductive material.
Preferably, organic solvent described in step (1) is n,N dimethylformamide.
Preferably, pore former described in step (1) is at least one of silicon, silica, polysilicon, silicon nitride；At
The particle diameter of hole agent is 50~500nm.Particle is excessive, cannot be coated well, and obtained spinning fibre is beading
Pattern；Particle is too small, and serious agglomeration can occur for voiding-agent particle, cannot be dispersed well.
Preferably, the mass ratio of polyacrylonitrile described in step (1) and pore former is (0.5~0.8): (0.05~0.1).
Preferably, water-soluble high-molecular material described in step (2) is polyvinyl alcohol, polyvinylpyrrolidone, alginic acid
Sodium or hyaluronic acid.
Preferably, electrostatic spinning described in step (3) refers to coaxial electrostatic spinning or microfluid electrostatic spinning.
Preferably, the time that water-bath described in step (4) is impregnated is 2~4h；The time of the freeze-drying is 12-24h.
Water-bath soaking time is less than 2h, then can not dissolve sandwich layer component, and the bubble time is greater than 4h, then subsequent sublimation drying is long, moisture
It possibly can not completely remove.
Preferably, step (5) Pre oxidation is 200~400 DEG C, and soaking time is 0.5~10h；The carburizing temperature
Be 550~1100 DEG C, soaking time be 1~for 24 hours, heating rate be 0.1~10 DEG C/min, specific gas flow rate be 5~500ml/
Min, inert atmosphere are argon gas or nitrogen.
It is highly preferred that the temperature of pre-oxidation described in step (5) is 250~280 DEG C, soaking time is 2~2.5h, heating
Rate is 2~3 DEG C/min.If heating rate, less than 2 DEG C/min, the time pre-oxidized is too long；If heating rate be greater than 3 DEG C/
Side reaction then may first occur for min.The temperature of pre-oxidation cannot then complete pre-oxidation less than 200 DEG C；If pre-oxidation
Temperature be greater than 400 DEG C, then fiber may be melted or be burnt because of overheat.The temperature of the carbonization treatment is 600~650
DEG C, carbonization time is 3~6h.If carburizing temperature, less than 600 DEG C, the time is less than 3h, then the non-carbon elements such as H, N can not be from fiber
Abjection is clean；If carburizing temperature is greater than 650 DEG C, the time is greater than 6h, then the intensity of carbon fiber can decline, and influence chemical property
It plays.
Preferably, etching processing described in step (5) refer to by reactive ion etching, inductively coupled plasma etching or
Wet etching.
A kind of porous hollow fiber conductive material, is prepared by the above method.
Further, the fibre diameter of the porous hollow fiber conductive material is 100~500nm, specific surface area 600
~700m2/ g, conductivity are 0.01~0.10s/cm.
Compared with prior art, the invention has the following advantages and beneficial effects:
(1) by coaxial electrostatic spinning or microfluid electrostatic spinning, it is equipped with water-bath immersion and freeze-drying process, it can
The skin-core structure for guaranteeing conductive material, keeps the fiber shape structure of material, is conducive to following process as types of functionality dress ornament.
(2) porous structure is prepared by pre-oxidation, carbonization and etching processing, while removes nonconducting related component, dropped
Low resistivity of material improves the electric conductivity of material.
(3) by preparing porous hollow fiber, gathering for charge is reduced by skin-core structure and porous structure, reduces charge
Density improves the antistatic durability of material.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
The polyacrylonitrile of 0.5g is added in the n,N dimethylformamide of 5ml, wait be added after being completely dissolved
0.05g diameter is the Si and SiO of 100nm2Particle is sufficiently mixed and stirs evenly, and obtains cortex solution；By the polyvinyl alcohol of 0.1g
It is added in the deionized water of 1ml, obtains sandwich layer solution；Cortex solution and sandwich layer solution are obtained by coaxial electrostatic spinning
With skin-core structure complex fiber material, complex fiber material is then impregnated into 2h by water-bath, is transferred to vacuum freeze drying
In case, it is freeze-dried 12h, the sandwich layer ingredient of skin-core structure complex fiber material is removed, obtains hollow fiber material；It will obtain
Hollow fiber material in tube furnace under nitrogen atmosphere experience pre-oxidation (250 DEG C, 2h) and be carbonized (600 DEG C, 4h) process, and
Use reactive ion etching Si and SiO2Particle obtains porous hollow fiber conductive material.
The doughnut conductive material fibre diameter that the present embodiment obtains is 500nm, specific surface area 700m2/ g, conductance
Rate is 0.10s/cm, reduces gathering for charge by skin-core structure and porous structure, reduces charge density, improve material prevent it is quiet
Electrical endurance.
Embodiment 2
The polyacrylonitrile of 0.8g is added in the n,N dimethylformamide of 10ml, wait be added after being completely dissolved
0.1g diameter is the silicon nitride of 50nm, is sufficiently mixed and stirs evenly, obtains cortex solution；The sodium alginate of 1g is added to 5ml
Deionized water in, obtain sandwich layer solution；Cortex solution and sandwich layer solution are obtained by microfluid electrostatic spinning with skin
Cored structure complex fiber material；Then complex fiber material is impregnated into 4h by water-bath, is transferred in vacuum freezing drying oven,
Freeze-drying for 24 hours, removes the sandwich layer ingredient of skin-core structure complex fiber material, obtains hollow fiber material；It is hollow by what is obtained
Fibrous material experience pre-oxidation (200 DEG C, 10h) and (the 550 DEG C, for 24 hours) process that is carbonized under nitrogen atmosphere in tube furnace, and use
Inductively ion etching silicon nitride particle obtains porous hollow fiber conductive material.
The doughnut conductive material fibre diameter that the present embodiment obtains is 100nm, specific surface area 600m2/ g, conductance
Rate is 0.01s/cm, reduces gathering for charge by skin-core structure and porous structure, reduces charge density, improve material prevent it is quiet
Electrical endurance.
Embodiment 3
The polyacrylonitrile of 0.6g is added in the n,N dimethylformamide of 8ml, wait be added after being completely dissolved
0.08g particle diameter is the polysilicon of 500nm, is sufficiently mixed and stirs evenly, obtains cortex solution；By the polyvinyl pyrrole of 0.5g
Alkanone is added in the deionized water of 3ml, obtains sandwich layer solution；Cortex solution and sandwich layer solution are passed through into coaxial electrostatic spinning
It obtains with skin-core structure complex fiber material；Then complex fiber material is impregnated into 3h by water-bath, is transferred to vacuum refrigeration
In drying box, it is freeze-dried 18h, the sandwich layer ingredient of skin-core structure complex fiber material is removed, obtains hollow fiber material；It will
Obtained hollow fiber material experience pre-oxidation (400 DEG C, 0.5h) and carbonization (1100 DEG C, 1h) under argon atmosphere in tube furnace
Process, and wet etching polycrysalline silcon is used, obtain porous hollow fiber conductive material.
The doughnut conductive material fibre diameter that the present embodiment obtains is 300nm, specific surface area 650m2/ g, conductance
Rate is 0.05s/cm, reduces gathering for charge by skin-core structure and porous structure, reduces charge density, improve material prevent it is quiet
Electrical endurance.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of porous hollow fiber conductive material, it is characterised in that including following preparation step:
(1) preparation of cortex solution: polyacrylonitrile is dissolved in organic solvent, and pore former is then added and is uniformly mixed,
Obtain cortex solution；
(2) preparation of sandwich layer solution: water-soluble high-molecular material is dissolved in deionized water, obtains sandwich layer solution；
(3) cortex solution and sandwich layer solution are obtained by electrostatic spinning with skin-core structure complex fiber material；
(4) there will be skin-core structure complex fiber material by water-bath immersion and freeze-drying process, it is compound to remove skin-core structure
The sandwich layer ingredient of fibrous material, obtains hollow fiber material；
(5) then hollow fiber material is performed etching under an inert atmosphere by pre-oxidation and carbonization treatment for pore former
Processing, obtains porous hollow fiber conductive material.
2. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(1) organic solvent described in is n,N dimethylformamide.
3. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(1) pore former described in is at least one of silicon, silica, polysilicon, silicon nitride；The particle diameter of pore former be 50~
500nm。
4. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(1) mass ratio of polyacrylonitrile described in and pore former is (0.5~0.8): (0.05~0.1).
5. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(2) water-soluble high-molecular material described in is polyvinyl alcohol, polyvinylpyrrolidone, sodium alginate or hyaluronic acid.
6. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(3) electrostatic spinning described in refers to coaxial electrostatic spinning or microfluid electrostatic spinning.
7. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(4) time that water-bath described in is impregnated is 2~4h；The time of the freeze-drying be 12~for 24 hours.
8. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(5) Pre oxidation is 200~400 DEG C, and soaking time is 0.5~10h；The carburizing temperature is 550~1100 DEG C, when heat preservation
Between for 1~for 24 hours, heating rate is 0.1~10 DEG C/min, and specific gas flow rate is 5~500ml/min；Inert atmosphere be argon gas or
Nitrogen.
9. a kind of preparation method of porous hollow fiber conductive material according to claim 1, it is characterised in that: step
(5) etching processing described in refers to through reactive ion etching, inductively coupled plasma etching or wet etching.
10. a kind of porous hollow fiber conductive material, is prepared by method according to any one of claims 1 to 9；It is described
The fibre diameter of porous hollow fiber conductive material is 100~500nm, and specific surface area is 600~700m2/ g, conductivity are
0.01~0.10s/cm.
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Cited By (11)
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| CN110055622A (en) * | 2019-04-04 | 2019-07-26 | 东华大学 | A kind of preparation method of hollow structure porous carbon nanofiber |
| CN110112405A (en) * | 2019-05-29 | 2019-08-09 | 哈尔滨理工大学 | A kind of core-shell structure silicon/carbon fiber flexible combination electrode material and the preparation method and application thereof |
| CN110468469A (en) * | 2019-09-03 | 2019-11-19 | 黑龙江中医药大学 | One seed coat layer sandwich layer containing pore-foaming agent carries the preparation method of the coaxial electrostatic spinning silk fiber of medicine |
| CN110923924A (en) * | 2019-11-21 | 2020-03-27 | 东华大学 | Device and method for preparing photo-thermal water evaporation nanofiber knitted assembly |
| CN111097295A (en) * | 2019-12-19 | 2020-05-05 | 五邑大学 | Unidirectional moisture-conducting micro-nanofiber membrane with hollow nano-wicking pore channels and preparation method thereof |
| CN111188095A (en) * | 2020-01-08 | 2020-05-22 | 苏州大学 | Triangular hollow porous fiber and preparation method thereof |
| CN111235698A (en) * | 2020-03-24 | 2020-06-05 | 北华大学 | Preparation method and application of nitrogen-doped porous carbon fiber material |
| CN112899816A (en) * | 2021-01-26 | 2021-06-04 | 无锡优佳无纺科技有限公司 | Hollow polypropylene fiber for non-woven fabric and preparation method thereof |
| CN112968154A (en) * | 2021-02-01 | 2021-06-15 | 武汉大学 | Conductive composite material, preparation method thereof and application thereof in lithium ion battery electrode |
| CN113073426A (en) * | 2021-02-25 | 2021-07-06 | 东华大学 | Porous multi-hollow flexible composite nanofiber membrane material and preparation method thereof |
| CN114481357A (en) * | 2021-12-29 | 2022-05-13 | 武汉知朵科技有限公司 | Microstructure fiber and preparation method thereof |
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| CN110055622A (en) * | 2019-04-04 | 2019-07-26 | 东华大学 | A kind of preparation method of hollow structure porous carbon nanofiber |
| CN110112405B (en) * | 2019-05-29 | 2021-05-18 | 哈尔滨理工大学 | Core-shell structure silicon/carbon fiber flexible composite electrode material and preparation method and application thereof |
| CN110112405A (en) * | 2019-05-29 | 2019-08-09 | 哈尔滨理工大学 | A kind of core-shell structure silicon/carbon fiber flexible combination electrode material and the preparation method and application thereof |
| CN110468469A (en) * | 2019-09-03 | 2019-11-19 | 黑龙江中医药大学 | One seed coat layer sandwich layer containing pore-foaming agent carries the preparation method of the coaxial electrostatic spinning silk fiber of medicine |
| CN110923924B (en) * | 2019-11-21 | 2021-06-11 | 东华大学 | Device and method for preparing photo-thermal water evaporation nanofiber knitted assembly |
| CN110923924A (en) * | 2019-11-21 | 2020-03-27 | 东华大学 | Device and method for preparing photo-thermal water evaporation nanofiber knitted assembly |
| CN111097295A (en) * | 2019-12-19 | 2020-05-05 | 五邑大学 | Unidirectional moisture-conducting micro-nanofiber membrane with hollow nano-wicking pore channels and preparation method thereof |
| CN111188095A (en) * | 2020-01-08 | 2020-05-22 | 苏州大学 | Triangular hollow porous fiber and preparation method thereof |
| CN111235698A (en) * | 2020-03-24 | 2020-06-05 | 北华大学 | Preparation method and application of nitrogen-doped porous carbon fiber material |
| CN112899816A (en) * | 2021-01-26 | 2021-06-04 | 无锡优佳无纺科技有限公司 | Hollow polypropylene fiber for non-woven fabric and preparation method thereof |
| CN112968154A (en) * | 2021-02-01 | 2021-06-15 | 武汉大学 | Conductive composite material, preparation method thereof and application thereof in lithium ion battery electrode |
| CN113073426A (en) * | 2021-02-25 | 2021-07-06 | 东华大学 | Porous multi-hollow flexible composite nanofiber membrane material and preparation method thereof |
| CN113073426B (en) * | 2021-02-25 | 2022-05-31 | 东华大学 | Porous multi-hollow flexible composite nanofiber membrane material and preparation method thereof |
| CN114481357A (en) * | 2021-12-29 | 2022-05-13 | 武汉知朵科技有限公司 | Microstructure fiber and preparation method thereof |
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