CN108330679A - A kind of preparation method of graphene coated conductive fiber - Google Patents
A kind of preparation method of graphene coated conductive fiber Download PDFInfo
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- CN108330679A CN108330679A CN201710045725.6A CN201710045725A CN108330679A CN 108330679 A CN108330679 A CN 108330679A CN 201710045725 A CN201710045725 A CN 201710045725A CN 108330679 A CN108330679 A CN 108330679A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/42—Coatings containing inorganic materials
- C03C25/44—Carbon, e.g. graphite
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention belongs to Carbon Materials and composite material research field, specially a kind of preparation method of graphene coated conductive fiber, it is used as presoma by the way that the graphene hydrosol is made in graphene oxide reduction, it recycles dip-coating method that graphene uniform is coated on fiber, and the process can be repeated as many times.After drying, complete continuous graphene film is covered in fiber surface, obtains graphene coated conductive fiber.Meanwhile being shunk when colloidal sol drying and dehydrating, graphite ene coatings can be closely overlaid on fiber surface by the pressure generated in contraction process, it is made to be firmly combined with fiber, not easily to fall off.It mutually overlaps, be connected between fiber surface, graphene sheet layer, form conductive coating, the electric conductivity of fiber can be obviously improved.Above-mentioned fibrous composite has good electric conductivity, can be used for eliminating electrostatic or electromagnetic shielding, gathers around and have broad application prospects.The present invention has many advantages, such as that preparation process is simple, properties of product are controllable, is suitble to large-scale production.
Description
Technical field
The invention belongs to Carbon Materials and composite material research field, specially a kind of preparation of graphene coated conductive fiber
Method.
Background technology
With industrial development, electrostatic and electromagnetic radiation are to the normal work of electronic equipment and the physiology of the mankind
Health brings many negative effects.Since the antistatic effect of conductive fiber is notable, and after conductivity reaches a certain level,
Just there is excellent electro-magnetic screen function, the development and application of conductive fiber to be increasingly taken seriously.
Coating is a kind of method preparing conductive fiber, and common method is to coat carbon black on general fibre surface.It applies
Layer method may be used adhesive and carbon black be bonded in fiber surface, or directly by fiber surface fast softening and and carbon black
Bonding.The shortcomings that this method is that carbon black is easy to fall off, and carbon black is not easy to be uniformly distributed in fiber surface.In addition, due to bonding
The electric conductivity of the presence of agent, conductive coating can also be affected.
Since graphene is prepared in first time in 2004, the excellent physical property of graphene receives numerous scholars'
Extensive concern.Graphene has excellent electric conductivity, because only that one layer of atom, the movement of electronics is limited in a plane
On, the movement velocity of electronics wherein can reach the 1/300 of the light velocity, considerably beyond movement speed of the electronics in general conductor
Degree.The Theory Conductivity of graphene may be up to 108Ω/m is presently found best material conductive at room temperature, at room temperature
Resistance value only has 2/3rds of copper.Meanwhile graphene has very high radius-thickness ratio (up to 5000 or more) and specific surface area (reason
It is up to 2600m by value2/ g), the two-dimension plane structure of graphene makes it be more easy to constitute conductive mesh than zero dimension or one-dimensional electric material
Network.Exactly because graphene has these above-mentioned excellent performances, it is made to present good application prospect in electricity field.
The high conductivity of graphene and high radius-thickness ratio become fabulous conductive coating materials.It is coated in different matrix
Graphene film, you can assign encapsulated material certain electric conductivity.Meanwhile graphene is located at the outer surface of basis material,
The mechanics of basis material or other performances will not be had an impact.Dip-coating method is uniformly to coat colloidal sol-Gel Precursor
Graphene can be closely evenly coated at by using dip-coating method by fiber surface in a kind of method of substrate surface, and
Coating layer thickness can be regulated and controled by regulation technology parameter.Filamentary conductive after cladding is increased dramatically, and has antistatic
Or the potential application in electromagnetic shielding field.
In conclusion graphene coated can not be reduced its power in fiber surface while effective fiber electric conductivity
Performance is learned, preparing graphene coated conductive fiber has important practical significance.
Invention content
The purpose of the present invention is to provide a kind of preparation method of graphene coated conductive fiber, by by graphene uniform
It is coated on fiber surface, using the high conductivity of graphene, assigns fibrous material electric conductivity, current utter misery method preparation is solved and leads
Existing carbon black coating is uneven when electric fiber, caducous problem；This method is simple for process, is suitble to large-scale production.
The technical scheme is that：
A kind of preparation method of graphene coated conductive fiber, graphene is close, in the graphene coated conductive fiber
The even outer surface for being coated on fiber, processing procedure are before being with the graphene hydrosol being prepared by graphene oxide water solution
Body is driven, using Best-Effort request technique, the graphene hydrosol is coated to by fiber surface by Best-Effort request device, after drying and dewatering
Obtain graphene coated conductive fiber.
The graphene oxide water solution be by graphite oxide or graphene oxide powder with 1~5mg/ml addition go from
In sub- water, 15~30min of ultrasonic disperse is obtained.
The graphene hydrosol is by being quantitatively adding reducing agent into graphene oxide water solution, also by chemistry
Original obtains.
The graphene hydrosol preparation method is：A concentration of 80% hydration is added dropwise in graphene oxide water solution
Hydrazine solution, additive amount are 0.5~1.5wt% of graphene oxide water solution, and 3~5h is heated at 40~60 DEG C.
Used fiber is glass fibre, carbon fiber or organic fiber, and used fibre diameter is 10~40 μm.
The Best-Effort request device includes：Liquid bath, fixed pulley I, fixed pulley II, fixed pulley III are equipped with graphite in liquid bath
The alkene hydrosol, fiber to be covered forms the fiber of coated graphite alkene after graphene hydrosol Best-Effort request, in fiber to be covered
Channel on setting fixed pulley I, fixed pulley II, fixed pulley III, fixed pulley II is set in the graphene hydrosol, and graphene is water-soluble
The liquid level of glue is higher than the rotary shaft of fixed pulley II, and fixed pulley I, fixed pulley III are located at the top of liquid bath.
In the Best-Effort request device, a diameter of 3~15cm of pulley, the tangent line between fixed pulley II and fixed pulley III
Angle with horizontal plane is 75~90 °.
The fiber is at the uniform velocity advanced, and speed is 0.1~0.5m/s, and Best-Effort request number is 1~20 time.
The thickness of the graphite ene coatings is 0.5~10 μm, the volume conductance of graphene coated fiber is 0.1~
10S/cm。
The present invention design philosophy be：
Graphene has many excellent properties as a kind of New Two Dimensional Carbon Materials.Because only that one layer of atom, electronics
Movement is limited in a plane, and the movement velocity of electronics wherein can reach the 1/300 of the light velocity, exist considerably beyond electronics
Movement velocity in general conductor.The Theory Conductivity of graphene may be up to 108Ω/m, be it is presently found at room temperature it is conductive most
Good material.A small amount of graphene is only added, once constitute effective conductive network, you can it is obviously improved the electric conductivity of material.
On the other hand, the two-dimensional structure of graphene makes it have the characteristic easily to form a film, and the π-π between graphene molecules make
With so that it is mutually overlapped between graphene two dimensional surface, the graphene film stable structure of formation is survivable.Such as using conjunction
Suitable method, is coated on other materials surface by graphene film, then can assign the material certain electric conductivity.Further, since oxygen
Graphite alkene can form colloidal sol or gel, its viscosity is improved it is not necessary that the substances such as adhesive are added in processing procedure.Therefore, with
Traditional carbon black coating process is compared, and more convenient preparation process can be used.
Colloidal sol-Gel Precursor can be evenly applied to substrate surface by dip-coating method, and processing can be repeated several times.
Using dip-coating method, graphene can be evenly coated at fiber surface with sol-gel state, drying is dehydrated, i.e.,
The fiber of graphene coated can be obtained.Graphite ene coatings not only improve the electric conductivity of fiber, while graphene also has quality
Gently, corrosion resistant feature can further protect fiber.
In conclusion the present invention proposes a kind of preparation method of graphene coated conductive fiber, that is, utilize dip-coating method
The graphene hydrosol is coated on fiber surface, then graphene coated conductive fiber is obtained through dehydration and drying.This method has system
The advantages that standby simple for process, properties of product are controllable, it is suitble to large-scale production.
Compared with prior art, the invention has the advantages that and advantageous effect：
(1) present invention has better electric conductivity and mechanical performance using graphene as conductive coating materials compared with carbon black.
(2) present invention is without carrying out fiber surface complicated processing, and easy to operation, all flows all can be in temperate condition
Lower progress.
(3) graphene coated fiber coat produced by the present invention is securely uniform, not easily to fall off, especially can be according to reality
It needs to set the thickness of graphite ene coatings.
(4) preparation process of graphite ene coatings proposed by the present invention is simple, it is not necessary that the substances such as adhesive are added, it is ensured that graphite
The high conductivity of alkene is not weakened so that the filamentary conductive coated is substantially improved.
(5) present invention has many advantages, such as that preparation process is simple, and performance is controllable, is suitble to large-scale production.
Description of the drawings
Fig. 1 is graphene hydrosol Best-Effort request device used in the present invention.In figure, 1 fiber to be covered；2 liquid baths；3
Fixed pulley I；The 4 graphene hydrosols；5 fixed pulleys II；6 fixed pulleys III；The fiber of 7 coated graphite alkene.
Fig. 2 be Best-Effort request of the present invention during graphene coated fiber surface process schematic.Wherein, (a) oxygen
Graphite alkene solution；(b) the graphene hydrosol；(c) graphene is coated in fiber surface.
Fig. 3 is graphene coated conductive glass fibre stereoscan photograph prepared in the embodiment of the present invention 1.
Fig. 4 is graphene coated conductive glass fibre stereoscan photograph prepared in the embodiment of the present invention 2.
Fig. 5 is graphene coated conductive glass fibre stereoscan photograph prepared in the embodiment of the present invention 3.
Fig. 6 is graphene coated conductive glass fibre stereoscan photograph prepared in the embodiment of the present invention 4.
Fig. 7 is the stereoscan photograph of handled glass fibre in comparative example 1 of the present invention.
Fig. 8 is the stereoscan photograph of handled glass fibre in comparative example 2 of the present invention.
Specific implementation mode
As shown in Figure 1, graphene hydrosol Best-Effort request device used in the present invention includes mainly：Liquid bath 2, fixed pulley
I 3, fixed pulley II 5, fixed pulley III 6 etc., concrete structure is as follows：The graphene hydrosol 4 is equipped in liquid bath 2, fiber 1 to be covered passes through
The fiber 7 that coated graphite alkene is formed after 4 Best-Effort request of the graphene hydrosol, is arranged fixed pulley I on the channel of fiber 1 to be covered
3, fixed pulley II 5, fixed pulley III 6, fixed pulley II 5 are set in the graphene hydrosol 4, and the liquid level of the graphene hydrosol need to be higher than
The rotary shaft of fixed pulley II 5, fixed pulley I 3, fixed pulley III 6 are located at the top of liquid bath 2.
In a specific embodiment, the present invention configures graphene oxide first in the method for fiber surface coated graphite alkene
Aqueous solution, and be the graphene hydrosol by graphene oxide water solution processing, while forming the hydrosol, graphene oxide quilt
It is reduced to redox graphene.Graphene gel is then evenly applied to fiber using Best-Effort request device shown in FIG. 1
The fiber of coated graphite alkene is finally dried in surface.As shown in Fig. 2, it is as follows：
1. the preparation of the graphene hydrosol
Graphite oxide or graphene oxide are added with 1~5mg/ml in deionized water, 15~30min of ultrasonic disperse is obtained
To the graphene oxide water solution of stable and uniform.A concentration of 80wt% of 0.5~1.5wt% is added dropwise into graphene oxide solution
Hydrazine hydrate solution, heating 4h is stood after stirring evenly at 50 DEG C, the graphene hydrosol can be obtained.
2. the preparation of graphene coated conductive fiber
Best-Effort request device used in the present invention is as shown in Figure 1, technical parameter is as follows：The specification of fixed pulley I/II/III
It can be the same or different, diameter must be more than 3cm；The water-soluble glue liquid surface of graphene must be higher than the rotation of fixed pulley II in liquid bath
Axis；Fiber should keep vertical, tangent line (the i.e. fiber between fixed pulley II and fixed pulley III between fixed pulley II and fixed pulley III
Residing straight line) angle between horizontal plane cannot be less than 75 °, and the speed that fiber is advanced is 0.1~0.5m/s.
Fibre bundle is arranged according to shown in Fig. 1, passes through fixed pulley I/II/III successively, is finally collected in end.In room temperature
Under, fiber movement is drawn, fiber is by liquid gas two-phase interface, and when getting into the air, the graphene hydrosol can be coated on fiber
On, which can be described by Landau-Levich equations.After cladding process is as shown in Fig. 2, collect, drying processing (is being dried
60 DEG C of drying 1h in case), you can obtain uniform graphene coated conductive fiber.
To increase the thickness of graphite ene coatings, Best-Effort request process may be repeated 1~20 time, finally obtain with certain
Electric conductivity, specific thicknesses, uniform graphene coated conductive fiber.
In order to illustrate more clearly of technical scheme of the present invention, it is described in further detail with reference to embodiment.
Embodiment 1
200mg graphite oxides are taken, are added in 200ml deionized waters, ultrasonic disperse 20min obtains graphene oxide water
Solution.The hydrazine hydrate aqueous solution of a concentration of 80wt% of 2ml is added dropwise into graphene oxide water solution, stirs evenly and is placed on 50 DEG C
4h is heated in baking oven, and the obtained graphene hydrosol is poured into the liquid bath of Fig. 1.
Glass fibre is arranged as shown in Figure 1, with the speed drawing fiber movement of 0.3m/s, after Best-Effort request at 60 DEG C
1h is dried, obtains graphene coated conductive glass fibre, stereoscan photograph is as shown in figure 3, utilize graphite made from this method
Ene coatings electroconductive glass fibre, about 23.6 μm of diameter, volume conductance about 0.11S/cm.
Embodiment 2
Difference from Example 1 is, carries out 3 Best-Effort request processes to glass fibre, obtains graphite ene coatings and lead
Electric glass fibre, stereoscan photograph is as shown in figure 4, utilize graphene coated conductive glass fibre, diameter made from this method
About 25.5 μm, volume conductance about 1.5S/cm.
Embodiment 3
Difference from Example 1 is, carries out 10 Best-Effort request processes to glass fibre, obtains graphite ene coatings and lead
Electric glass fibre, stereoscan photograph is as shown in figure 5, utilize graphene coated conductive glass fibre, diameter made from this method
About 32.9 μm, volume conductance about 5.1S/cm.
Embodiment 4
Difference from Example 1 is, carries out 20 Best-Effort request processes to glass fibre, obtains graphite ene coatings and lead
Electric glass fibre, stereoscan photograph is as shown in fig. 6, utilize graphene coated conductive glass fibre, diameter made from this method
About 42.5 μm, volume conductance about 9.8S/cm.
Comparative example 1
Without using dip-coating method, only the graphene hydrosol is combined with glass fibre by mechanical agitation, wherein graphite
The preparation process of the alkene hydrosol is with embodiment 1, and the stereoscan photograph of fiber using this method as shown in fig. 7, be made after processing
Graphene and mixture of glass fibers, diameter is uneven to be determined, because graphene does not form connected network, therefore non-conductive.
Comparative example 2
The hydrosol is not made in graphene, Best-Effort request, the system of graphene aqueous solution are carried out only in graphene aqueous solution
Standby and Best-Effort request process is with embodiment 1, and the stereoscan photograph of fiber using this method as shown in figure 8, be made after processing
Graphene and mixture of glass fibers, about 22.7 μm of diameter, because graphene is uncoated on fiber, therefore non-conductive.
Embodiment and comparative example the result shows that, the present invention can be effectively by the graphene hydrosol by dip-coating method
It is coated to fiber surface, obtained graphene uniform coating thickness, and can assign fibrous material certain electric conductivity.At this
In the process, the formation film that the hydrosol is conducive to graphene is made in graphene, and Best-Effort request process can be equal by graphene
Even to be coated on fiber, Neither of the two can be dispensed.
In addition, the present invention utilizes the unique two-dimensional nanostructure of graphene, pass through above preparation process so that graphene
The conductive network being uniformly connected to is formed between lamella, graphene coated conductive fibre morphology obtained is uniform, uniform coating thickness
Controllably, it is suitble to large-scale production.
Claims (9)
1. a kind of preparation method of graphene coated conductive fiber, which is characterized in that graphite in the graphene coated conductive fiber
Alkene is close, is evenly coated at the outer surface of fiber, and processing procedure is the graphene to be prepared by graphene oxide water solution
The hydrosol is presoma, and using Best-Effort request technique, the graphene hydrosol is coated to fiber surface by Best-Effort request device,
Graphene coated conductive fiber is obtained after drying and dewatering.
2. the preparation method of graphene coated conductive fiber described in accordance with the claim 1, which is characterized in that the oxidation stone
Black aqueous solution is added in deionized water with 1~5mg/ml by graphite oxide or graphene oxide powder, ultrasonic disperse 15~
30min is obtained.
3. the preparation method of graphene coated conductive fiber described in accordance with the claim 1, which is characterized in that the graphene
The hydrosol is obtained by electronation by being quantitatively adding reducing agent into graphene oxide water solution.
4. according to the preparation method of the graphene coated conductive fiber described in claims 1 or 2 or 3, which is characterized in that described
Graphene hydrosol preparation method is：A concentration of 80% hydrazine hydrate solution, additive amount are added dropwise in graphene oxide water solution
For 0.5~1.5wt% of graphene oxide water solution, 3~5h is heated at 40~60 DEG C.
5. the preparation method of graphene coated conductive fiber described in accordance with the claim 1, which is characterized in that used fiber
For glass fibre, carbon fiber or organic fiber, used fibre diameter is 10~40 μm.
6. the preparation method of graphene coated conductive fiber described in accordance with the claim 1, which is characterized in that the dipping carries
Drawing device includes：Liquid bath, fixed pulley I, fixed pulley II, fixed pulley III are equipped with the graphene hydrosol, fiber warp to be covered in liquid bath
Fixed pulley I is arranged on the channel of fiber to be covered, determines for the fiber that coated graphite alkene is formed after graphene hydrosol Best-Effort request
Pulley II, fixed pulley III, fixed pulley II are set in the graphene hydrosol, and the liquid level of the graphene hydrosol is higher than fixed pulley II
Rotary shaft, fixed pulley I, fixed pulley III are located at the top of liquid bath.
7. the preparation method of graphene coated conductive fiber according to claim 6, which is characterized in that the dipping carries
In drawing device, a diameter of 3~15cm of pulley, tangent line angle with horizontal plane between fixed pulley II and fixed pulley III is 75~
90°。
8. the preparation method of graphene coated conductive fiber described in accordance with the claim 1, which is characterized in that the fiber is even
Speed is advanced, and speed is 0.1~0.5m/s, and Best-Effort request number is 1~20 time.
9. the preparation method of graphene coated conductive fiber described in accordance with the claim 1, which is characterized in that the graphene
The thickness of coating is 0.5~10 μm, and the volume conductance of graphene coated fiber is 0.1~10S/cm.
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| CN109179384A (en) * | 2018-09-11 | 2019-01-11 | 太原理工大学 | A kind of high-density graphite alkene and preparation method thereof |
| CN109322149A (en) * | 2018-09-29 | 2019-02-12 | 南京工业大学 | A kind of preparation method of degradable, multicolor luminous fiber |
| CN109594327A (en) * | 2018-12-06 | 2019-04-09 | 武汉纺织大学 | A kind of preparation method of fiber base graphene conductive material |
| CN111501334A (en) * | 2020-06-08 | 2020-08-07 | 北京石墨烯研究院 | Graphene compound and preparation method thereof |
| CN111549335A (en) * | 2020-05-09 | 2020-08-18 | 江苏匀超环保科技有限公司 | Graphene coating on surface of metal and carbon-based material electrode and preparation method thereof |
| CN114673004A (en) * | 2022-05-17 | 2022-06-28 | 中国热带农业科学院农产品加工研究所 | Preparation method of graphene antibacterial down feather |
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| CN109594327A (en) * | 2018-12-06 | 2019-04-09 | 武汉纺织大学 | A kind of preparation method of fiber base graphene conductive material |
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