CN105839203B - Utilize the three-dimensional porous yarn and preparation method thereof of Electrospinning preparation - Google Patents
Utilize the three-dimensional porous yarn and preparation method thereof of Electrospinning preparation Download PDFInfo
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- CN105839203B CN105839203B CN201610273756.2A CN201610273756A CN105839203B CN 105839203 B CN105839203 B CN 105839203B CN 201610273756 A CN201610273756 A CN 201610273756A CN 105839203 B CN105839203 B CN 105839203B
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- copper wire
- needle tubing
- capillary needle
- yarn
- conductive capillary
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Classifications
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- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- 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
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a kind of three-dimensional porous yarns and preparation method thereof using Electrospinning preparation.This method is to collect polymer or polymer composite fibrous prepared by Electrospun as supporter using rotation fiber, and three-dimensional porous yarn is prepared by subsequent processing.Preparation method of the invention can make yarn molding quickly direct, and the mobile phone molding of this method nano material for being suitble to all high-voltage electrostatic spinnings that can prepare；And the yarn that the present invention is prepared has the network structure of mutual connection, is advantageously implemented big conductivity.It is filled between the nanofiber by the hole largely to communicate with one another, is conducive to the diffusion of liquid such as electrolyte in the electrodes.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of three-dimensional using Electrospinning preparation is more
Hole yarn and preparation method thereof.
Background technique
Early in the 1960s, the thought and blank of wearable smart machine have occurred.In recent years, with information skill
The fast development of art, nanotechnology, material science, energy storage technology etc., wearable device have initially entered the fast-developing stage,
Its form and function start to become diversification, gradually show in the numerous areas such as industry, medical treatment, military, education, amusement important
Researching value and application potential.The development of wearable device is that energy resource supply device proposes more requirements: can be woven, gently
Matter, large capacity, high magnification, high stability etc..
The method for currently preparing wire electrode includes wet spinning technology, dry spinning, the technologies such as confinement hydro-thermal.Use wet process
Spinning or dry spinning technology prepare yarn and there are certain requirements to the physicochemical properties of material, and the material of some function admirables is past
Toward the condition for being unsatisfactory for dry spinning and wet spinning.As dry spinning need material be polymer and have certain viscosity,
Molecular weight is sufficiently large, suitable electric conductivity and surface tension etc.；Wet spinning then utilizes material consolidating under certain chemical reactions
Change property to prepare yarn, is only suitable for meeting the material specifically chemically reacted.And confinement hydro-thermal method is in addition to being required to meet
Specific chemical reaction also needs reaction product to generate continuous colloidal sol or gel yarn.In addition, confinement hydro-thermal method is by confinement
The limitation of container, can not continuous production yarn.
As can be seen from the above analysis, the method for currently preparing yarn has its limitation, and explores new yarn system
Standby technology becomes a key technical problem of current field of nanometer material technology to replace or make up current techniques.The solution of the problem
It will certainly be provided for fields such as supercapacitor, lithium ion battery, lithium-sulfur cell, photoelectric chemical electrode, photocatalysis, pollutant absorption
New material preparation technology.
Summary of the invention
[technical problems to be solved]
Present invention aim to address above-mentioned prior art problems, and it is more to provide a kind of three-dimensional using Electrospinning preparation
Hole yarn and preparation method thereof.
[technical solution]
In order to reach above-mentioned technical effect, the present invention takes following technical scheme:
The present invention is by high-voltage electrostatic spinning technology, using special Electrospun wire drawing device --- and rotation fiber realizes yarn
The straight forming of line electrode is collected.
A kind of preparation method preparing three-dimensional porous yarn using Electrospinning, this method are using rotation fiber conduct
Supporter collects the polymer or polymer composite fibrous of Electrospun preparation, and three-dimensional porous yarn is prepared by subsequent processing
Line.
Further technical solution according to the present invention, the rotation fiber are the wires, cotton thread, change of diameter < 1cm
Learn fiber or glass fibre.
Further technical solution according to the present invention, the preferred carbon fiber of chemical fibre；The wire is titanium
Silk, steel wire, tantalum wire, copper wire or nickel wire.
Further technical solution according to the present invention, the rotary rpm of the rotation fiber are 0~20000rpm.
Further technical solution according to the present invention, the polymer or polymer composite fibrous including polyacrylonitrile
PAN, polyvinylpyrrolidone PVP, PVAC polyvinylalcohol, polyoxyethylene PEO, polyvinyl acetate PVAc, poly- 3,4- enedioxy
One of thiophene PEDOT, polyaniline are a variety of.
Further technical solution according to the present invention, the subsequent processing are to remove or do not remove rotation fiber, thereafter
Continuous processing includes that carbonization technique, in-situ polymerization, soda acid processing, photocuring, electronics or ion beam irradiation or radioactivity irradiate.
The above-mentioned preparation method for preparing three-dimensional porous yarn using Electrospinning is by Electrospun precursor solution quiet
Under conditions of voltage is 5~50kV, conductive capillary needle pore diameter is 0.5~0.8nm, with the flow velocity of 0.02~0.5mL/h
Outflow carries out Electrospun operation from conductive capillary needle tubing.
A kind of three-dimensional porous yarn, the three-dimensional porous yarn are prepared by above-mentioned preparation method.Gained yarn is by receiving
Rice fiber composition, the nanofiber form the network structure of mutual connection in structure, are advantageously implemented big conductivity.It is described
It is filled between nanofiber by the hole largely to communicate with one another, is conducive to the diffusion of liquid such as electrolyte in the electrodes.
The three-dimensional porous yarn is made of 1 μm of diameter < of nanofiber, by being mutually connected between the nanofiber
The hole of logical aperture > 10nm is filled.
A kind of application for the three-dimensional porous yarn being prepared according to above-mentioned preparation method, the three-dimensional porous yarn can be applied
In supercapacitor, lithium ion battery, lithium-sulfur cell, photoelectric chemical electrode, photocatalysis or pollutant adsorbing domain.
A kind of electric spinning device that above-mentioned preparation method uses, it includes high voltage power supply, conductive capillary needle tubing and gold
Belong to and collect plate, the positive and negative anodes of the high voltage power supply are connect with conductive capillary needle tubing, metal collection plate respectively, it is also wrapped
Rotation fiber is included, the rotation fiber is placed between conductive capillary needle tubing and metal collection plate, and the rotation is fine
The axis and metal collection platen parallel of dimension；The rotation fiber is placed in below conductive capillary needle tubing at 1~100cm, metal
Collect on plate at 0.1~100cm, and the rotation fiber at a distance from metal collection plate than itself and conductive hair
The distance of small needle tube is short；The rotation fiber can be connected or be not attached to metal collection plate.
It will be described in detail the present invention below.
Then the wire drawing device that the present invention is equipped using the fiber of rotation as high-voltage electrostatic spinning is prepared by Electrospun
The molding that winds realize yarn of the fiber in rotation fiber is collected.The high-voltage electrostatic spinning technology that the present invention uses is existing
Technology, the device used are also possible to existing apparatus, but conductive capillary needle tubing and metal in existing apparatus is needed to receive
Rotation fiber is set between collection plate.Specifically the preparation method is as follows: Electrospun precursor solution passes through conductive capillary needle
Pipe outflow, is drawn into nanofiber under the comprehensive functions such as high-voltage electrostatic field, solution viscous force, solution surface tension, gravity.
The high voltage electric field is applied on conductive capillary needle tubing and metal collection plate by high voltage power supply by conducting wire.The rotation
Turn supporter of the fiber as Electrospun product, can be removed after being successfully prepared and prepare hollow three-dimensional porous electrode, it can also
A part as electrode is not removed, plays carrier collection or increases mechanical performance.
[beneficial effect]
Compared with prior art, the present invention have it is below the utility model has the advantages that
Preparation method of the invention can make yarn molding quickly direct, and this method is suitble to all high-voltage electrostatic spinnings
The collection for the nano material that can be prepared forms；And the yarn that the present invention is prepared is made of nanofiber, the Nanowire
Dimension forms the network structure of mutual connection in structure, is advantageously implemented big conductivity.By a large amount of mutual between the nanofiber
The hole filling being connected, is conducive to the diffusion of liquid such as electrolyte in the electrodes.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of electric spinning device of the present invention；
Fig. 2 is the electron scanning micrograph of three-dimensional porous yarn prepared by the embodiment of the present invention 1.
Specific embodiment
Below with reference to the embodiment of the present invention, the invention will be further elaborated.
A kind of electric spinning device as shown in Figure 1, it includes high voltage power supply 4, conductive capillary needle tubing 2 and metal collection
Plate 6, the positive and negative anodes of the high voltage power supply 4 are connect with conductive capillary needle tubing 2, metal collection plate 6 respectively, it further includes
Rotation fiber 7, the rotation fiber 7 is placed between conductive capillary needle tubing 2 and metal collection plate 6, and the rotation
The axis and metal collection platen parallel of fiber；The rotation fiber is placed in below conductive capillary needle tubing at 1~100cm, is golden
Belong to and collecting on plate at 0.1~100cm, and the rotation fiber at a distance from metal collection plate than its with it is conductive
The distance of capillary needle tubing is short；The rotation fiber can be connected or be not attached to metal collection plate.
Prepared that specific step is as follows using the electric spinning device: Electrospun precursor solution 1 passes through conductive
Capillary needle tubing 2 flows out, and is drawn into and receives under the comprehensive functions such as high-voltage electrostatic field, solution viscous force, solution surface tension, gravity
Rice fiber 3.The high voltage electric field is applied to conductive capillary needle tubing 2 and metal collection plate by conducting wire 5 by high voltage power supply 4
On 6；The nanofiber 3 of Electrospun preparation is assembled under electric field action on metal collection plate 6, is placed in accumulation process
The winding of rotation fiber 7 on metal collection plate collects and forms yarn.
Following embodiment is prepared by above-mentioned electric spinning device.
Embodiment 1:
0.5g PAN is dissolved in 5mL dimethylformamide (DMF) and is used as Electrospun solution.Then with
The flow velocity of 0.2mL/h is flowed out from conductive capillary needle tubing, the rotation titanium silk that conductive capillary needle tubing and diameter are 300 microns
The distance between be 15cm, conductive capillary needle tubing to the distance between metal collection plate is 18cm, and rotation fiber is placed in gold
Belong to and collect the source 3cm on plate, rotate the axis of titanium silk and collects platen parallel, the conductive capillary needle tubing and high-voltage electricity
Source it is positive it is (negative) be extremely connected, metal collection plate and bearing (just) is connected.Apply between conductive capillary needle tubing and metal plate
The high pressure of 15kV.The revolving speed that control rotates Ti is 3000rpm.
The nanometer PAN nanofiber of the present embodiment Electrospun preparation falls on rotation titanium silk and is wound and is rolled in titanium silk table
Face forms PAN yarn.It is received to Ti/ carbon as shown in Figure 2 is obtained after the PAN yarn progress carbonization treatment of prepared titaniferous silk
Rice fiber yarn.
Product Ti/ carbon nano-fiber yarn can be applicable to yarn supercapacitor field, since the structure has simultaneously
The conductive network and electrolyte proliferation network of mutual connection, can significantly improve active material utilization, improve device specific capacity,
Energy density, power density.
Embodiment 2
0.5g PAN is dissolved in 5mL dimethylformamide (DMF) and is used as Electrospun solution.Then with
The flow velocity of 0.2mL/h is flowed out from conductive capillary needle tubing, the rotation copper wire that conductive capillary needle tubing and diameter are 300 microns
The distance between be 15cm, conductive capillary needle tubing to the distance between metal collection plate is 18cm, and rotation fiber is placed in gold
Belong to and collect the source 3cm on plate, rotate the axis of copper wire and collects platen parallel, the conductive capillary needle tubing and high-voltage electricity
Source it is positive it is (negative) be extremely connected, metal collection plate and bearing (just) is connected.Apply between conductive capillary needle tubing and metal plate
The high pressure of 15kV.The revolving speed of control rotation copper wire is 3000r/min.
The nanometer PAN nanofiber of the present embodiment Electrospun preparation falls on rotation copper wire and is wound and is rolled in copper wire table
Face forms PAN yarn.The prepared PAN yarn containing copper wire is carried out to obtain Cu/ carbon nano-fiber yarn after carbonization treatment.
Carbon nano-fiber yarn is obtained after eroding copper wire with nitric acid.
The hollow carbon nano-fibre yams can be applicable to the fields such as electro-catalysis, supercapacitor, since the structure has simultaneously
There are the conductive network and electrolyte proliferation network of mutual connection, active material utilization can be significantly improved, the electricity for improving device is urged
Change performance (to electro-catalysis) specific capacity, energy density, power density (supercapacitor).
Embodiment 3
0.5g PAN is dissolved in 5mL dimethylformamide (DMF) and is used as Electrospun solution.Then with
The flow velocity of 0.2mL/h is flowed out from conductive capillary needle tubing, the rotation copper wire that conductive capillary needle tubing and diameter are 400 microns
The distance between be 15cm, conductive capillary needle tubing to the distance between metal collection plate is 18cm, and rotation fiber is placed in gold
Belong to and collect the source 3cm on plate, rotate the axis of copper wire and collects platen parallel, the conductive capillary needle tubing and high-voltage electricity
Source it is positive it is (negative) be extremely connected, metal collection plate and bearing (just) is connected.Apply between conductive capillary needle tubing and metal plate
The high pressure of 15kV.The revolving speed of control rotation copper wire is 3000r/min.
The nanometer PAN nanofiber of the present embodiment Electrospun preparation falls on rotation carbon fiber bundle (by 7 microns of carbon fiber of diameter
Dimension composition, about 100 microns of diameter) on and be wound and be rolled in carbon fiber bundle surface formed PAN yarn.Carbon fiber is contained to prepared
The PAN yarn of dimension beam carries out obtaining carbon fiber bundle/carbon nano-fiber yarn after carbonization treatment.
The hollow carbon nano-fibre yams can be applicable to supercapacitor field, since the structure has mutual connection simultaneously
Conductive network and electrolyte proliferation network, can significantly improve active material utilization, and specific capacity, the energy for improving device are close
Degree, power density (supercapacitor).
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (1)
1. a kind of preparation method for preparing three-dimensional porous yarn using Electrospinning, it is characterised in that:
Electric spinning device is utilized, the electric spinning device includes high voltage power supply (4), conductive capillary needle tubing (2) and metal
Collect plate (6), the positive and negative anodes of the high voltage power supply (4) respectively with conductive capillary needle tubing (2), metal collection plate (6)
Connection, electric spinning device further include rotation copper wire (7), and the rotation copper wire (7) is placed in conductive capillary needle tubing (2) and metal
It collects between plate (6), and the axis and metal collection platen parallel of the rotation copper wire；The rotation copper wire and metal collection
The distance of plate than its at a distance from conductive capillary needle tubing it is short；The rotation copper wire can be connected with metal collection plate or
It is not attached to；
Specific step is as follows:
Electrospun precursor solution is flowed out by conductive capillary needle tubing, in high-voltage electrostatic field, solution viscous force, solution surface
Nanofiber is drawn under tension, gravity comprehensive function；It is applied by high voltage power supply (4) by conducting wire (5) high-voltage electrostatic field
It is added on conductive capillary needle tubing (2) and metal collection plate (6)；The nanofiber (3) of Electrospun preparation is in electric field action
Lower to assemble on metal collection plate (6), rotation copper wire (7) winding being placed on metal collection plate in accumulation process is collected
And form yarn；
0.5g PAN is dissolved in 5mL DMF as Electrospun precursor solution；Then with the flow velocity of 0.2mL/h from electrically conductive
Capillary needle tubing outflow, the distance between the rotation copper wire that conductive capillary needle tubing and diameter are 300 microns is 15cm, can be led
The capillary needle tubing of electricity is 18cm to the distance between metal collection plate, and rotation copper wire is placed in the source 3cm on metal collection plate,
It rotates the axis of copper wire and collects platen parallel, the conductive capillary needle tubing is connected with the positive or negative pole of high voltage power supply, gold
Belong to collecting board to be connected with cathode or anode；Apply the high pressure of 15kV between conductive capillary needle tubing and metal plate；Control
The revolving speed for rotating copper wire is 3000r/min；
The nanometer PAN nanofiber of Electrospun preparation falls on rotation copper wire and is wound and is rolled in copper wire surface and forms PAN yarn
Line；The prepared PAN yarn containing copper wire is carried out to obtain Cu/ carbon nano-fiber yarn after carbonization treatment；Corroded with nitric acid
Fall copper wire and obtains carbon nano-fiber yarn later.
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| Application Number | Priority Date | Filing Date | Title |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106299286B (en) * | 2016-09-08 | 2018-11-30 | 天津大学 | A kind of lithium-sulfur cell macromolecule composite positive pole and preparation method |
| CN106531474A (en) * | 2016-12-14 | 2017-03-22 | 中国工程物理研究院化工材料研究所 | Linear electrode and preparation method therefor by adopting electrospinning technique |
| CN109253740B (en) * | 2018-09-10 | 2021-02-12 | 中原工学院 | Capacitive sensor based on nanofiber core-spun yarn and preparation method thereof |
| CN109273273B (en) * | 2018-09-10 | 2020-09-04 | 中原工学院 | PAN-GO/PEDOT/PSS supercapacitor electrode material based on nanofiber yarn and preparation method thereof |
| CN214142625U (en) * | 2020-04-13 | 2021-09-07 | 广东三水合肥工业大学研究院 | Splicing electrostatic spinning equipment |
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| CN1472373A (en) * | 2003-03-28 | 2004-02-04 | 中国科学院长春应用化学研究所 | Rotary disc spinning process and apparatus |
| CN101664346A (en) * | 2009-09-02 | 2010-03-10 | 南通大学 | Artificial nerve graft prepared by electrostatic spinning and preparation method and special device thereof |
| CN102008755A (en) * | 2010-11-25 | 2011-04-13 | 武汉纺织大学 | Polyethylene terephthalate and polyurethane composite artificial blood vessel and preparation thereof |
| CN102912456A (en) * | 2011-08-04 | 2013-02-06 | 中国人民解放军装甲兵工程学院 | Method and system for preparing nanofiber coating on surface of yarn or fiber bundle |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100458946B1 (en) * | 2002-08-16 | 2004-12-03 | (주)삼신크리에이션 | Electrospinning apparatus for producing nanofiber and electrospinning nozzle pack for the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1472373A (en) * | 2003-03-28 | 2004-02-04 | 中国科学院长春应用化学研究所 | Rotary disc spinning process and apparatus |
| CN101664346A (en) * | 2009-09-02 | 2010-03-10 | 南通大学 | Artificial nerve graft prepared by electrostatic spinning and preparation method and special device thereof |
| CN102008755A (en) * | 2010-11-25 | 2011-04-13 | 武汉纺织大学 | Polyethylene terephthalate and polyurethane composite artificial blood vessel and preparation thereof |
| CN102912456A (en) * | 2011-08-04 | 2013-02-06 | 中国人民解放军装甲兵工程学院 | Method and system for preparing nanofiber coating on surface of yarn or fiber bundle |
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