CN106337215A - Carbon nanotube composite fiber and production method thereof - Google Patents
Carbon nanotube composite fiber and production method thereof Download PDFInfo
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- CN106337215A CN106337215A CN201610392946.6A CN201610392946A CN106337215A CN 106337215 A CN106337215 A CN 106337215A CN 201610392946 A CN201610392946 A CN 201610392946A CN 106337215 A CN106337215 A CN 106337215A
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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
-
- 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
- D01D5/12—Stretch-spinning methods
-
- 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
- D01F1/10—Other agents for modifying properties
-
- 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
Abstract
The invention discloses a carbon nanotube composite fiber and a production method thereof. The production method comprises the following steps: continuously pulling out a carbon nanotube film from a spinnable carbon nanotube array, keeping the carbon nanotube film in an open and flat state, allowing the carbon nanotube film to continuously and stably be in full contact with a liquid phase system including a selected substance to make the selected substance fill a gap among carbon nanotubes composing the carbon nanotube film or be attached to the surface of the carbon nanotubes composing the carbon nanotube film, and collecting the formed fiber in order to obtain the carbon nanotube composite fiber. The production method of the carbon nanotube composite fiber is simple and effective, is suitable for producing various composite fibers, can endow carbon nanotube fibers with abundant function characteristics through adding compounds without destroying the self performances of the carbon nanotube fibers, and also realizes continuous large-scale enforcement to make large-scale production manufacturing of the carbon nanotube composite fiber become possible.
Description
Technical field
The present invention relates to a kind of carbon nano tube composite fibre, particularly to a kind of carbon nano tube composite fibre and preparation method thereof, belong to
The micro- technical field of composite materials of nanometer.
Background technology
Since carbon nano-tube fibre was successfully prepared from 2002 by Tsing-Hua University scientific research personnel from carbon nano pipe array, obtain domestic
The extensive concern of outer research worker.Because CNT has the performances such as excellent power, heat, electricity, obtained by CNT assembling
Carbon nano-tube fibre also has excellent performance and wider application.
At present, the preparation method of the carbon nano-tube fibre of development includes array and reels off raw silk from cocoons method, floating catalytic vapour deposition process and solution
Spin processes etc..The tensile strength of prepared carbon nano-tube fibre, also up to more than 1.0gpa, meets most of components to material
The requirement of mechanical strength.With going deep into of the research to carbon nano-tube fibre, powerful becomes restriction carbon nano-tube fibre and is applied to
The main cause of wide range of areas.There are reports at present introduces feature object, to improve carbon nanometer in carbon nano-tube fibre
The feature of pipe fiber.For example, having been prepared carbon nano-tube fibre makes Graphene be attached to carbon nanometer by way of spraying or soaking
On pipe fiber.Although this method successfully Graphene is introduced in fiber, Graphene can only be attached at carbon nano tube surface, because
This is difficult to significantly improve the performance of carbon nano-tube fibre.Further, it is also possible to from CNT can be pulled out spinning carbon nano pipe array
Thin film, and by thinfilms in the round roller of fixed dimension and molten to carbon nano-tube film sprinkling or immersion graphene oxide in round roller
Then thin film is taken off winding or twists into threadiness, thus obtaining CNT/graphene oxide fiber by liquid.Although this method
Graphene can be introduced fibrous inside, but thin film size-constrained in round roller size, and be difficult to continuously implement on a large scale.
Content of the invention
Present invention is primarily targeted at providing a kind of carbon nano tube composite fibre and preparation method thereof, with overcome of the prior art not
Foot.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes:
Embodiments provide a kind of preparation method of carbon nano tube composite fibre, comprising: from can spinning carbon nano pipe array
In pull straight carbon nano-tube film, and make described carbon nano-tube film keep flattened state and continuously and stably with comprise to select material
Liquid-phase system be fully contacted so that described selected material be sufficient filling with form described carbon nano-tube film CNT between and/or
Integrated fibers are received, thus obtaining described CNT to be combined fibre after being attached to the carbon nano tube surface forming described carbon nano-tube film
Dimension.
In a preferred embodiment, described preparation method includes: makes described carbon nano-tube film abundant with described liquid-phase system
After contact, regather and twisting forms described fiber simultaneously.
In a preferred embodiment, described preparation method also includes: described carbon nano tube composite fibre is dried and high temperature
Process.
The embodiment of the present invention additionally provides a kind of carbon nano tube composite fibre, and it comprises complex root CNT and assembles the threadiness being formed
Structure and be at least dispersed in selected material in described filamentary structure, the most of carbon nanometer in this complex root CNT
Pipe is wound around along the axially continuous spiral extension of described composite fibre and mutually.
Compared with prior art, the invention has the advantages that the carbon nano-composite fiber preparation method providing is simply effective, applicable
In the preparation of multiple composite fibres, can be assigned by the addition of complex on the premise of not destroying carbon nanometer tube fiber performance itself
Give the functional characteristic that carbon nano-tube fibre is more rich, and can continuously implement on a large scale, make large-scale production manufacture CNT multiple
Condensating fiber is possibly realized.
Brief description
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, embodiment or prior art will be retouched below
In stating the accompanying drawing of required use be briefly described it should be apparent that, drawings in the following description be only the present invention described in
Some embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to these
Accompanying drawing obtains other accompanying drawings.
Fig. 1 is the schematic flow sheet of specific embodiment in the embodiment of the present invention 1；
Fig. 2 is the tensile property comparison diagram of carbon nano tube/graphene composite fibre and pure carbon nanotube fibers in the embodiment of the present invention 1；
Fig. 3 is that in the embodiment of the present invention 2, carbon nano tube/silver Nanocomposites fiber is compared with the electric conductivity of pure carbon nanotube fibers
Figure；
Fig. 4 is the tensile property ratio of post processing formula carbon nano tube/graphene composite fibre and pure carbon nanotube fibers in comparative example of the present invention
Relatively scheme.
Specific embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with the accompanying drawings the specific embodiment of the present invention is entered
Row describes in detail.The example of these preferred implementations is illustrated in the accompanying drawings.The basis describing shown in accompanying drawing and with reference to the accompanying drawings
The embodiment of invention is merely exemplary, and the present invention is not limited to these embodiments.
Here, also, it should be noted in order to avoid having obscured the present invention because of unnecessary details, illustrate only in the accompanying drawings
With the structure closely related according to the solution of the present invention and/or process step, and eliminate the other details little with relation of the present invention.
Embodiments provide a kind of preparation method of carbon nano tube composite fibre, comprising: from can spinning carbon nano pipe array
In pull straight carbon nano-tube film, and make described carbon nano-tube film keep flattened state and continuously and stably with comprise to select material
Liquid-phase system be fully contacted so that described selected material be sufficient filling with form described carbon nano-tube film CNT between and/or
Integrated fibers are received, thus obtaining described CNT to be combined fibre after being attached to the carbon nano tube surface forming described carbon nano-tube film
Dimension.Wherein, by described carbon nano-tube film is kept flattened state, the most carbon in this carbon nano-tube film can be made to receive
It is available for selecting the gap that material enters between mitron, and then beneficial to selecting the compound of material and CNT.
Further, described carbon nano-tube film is made to keep flattened state and with setting speed continuously and stably from described liquid-phase system
Pass through, receive integrated fibers afterwards.
Further, after so that described carbon nano-tube film and described liquid-phase system is fully contacted, regather and twisting forms institute simultaneously
State fiber.
More preferred, described liquid-phase system comprises solvent and is dissolved in and/or is dispersed in the selected material in described solvent.
More preferred, described solvent can be selected from any suitable solvent, including water and/or organic solvent.
It is more highly preferred to, described organic solvent includes ethanol, isopropanol, n, n- dimethylformamide, dimethyl sulfoxide, chloroform
Deng in any one or two or more combinations, but not limited to this.
More preferred, described selected material includes any suitable material, for example can be dissolved in described solvent material or can be equal
The even material being scattered in described solvent.
It is more highly preferred to, described selected material includes conjugated molecule (such as pyrene, poly- 3- hexyl thiophene, polypyrrole etc.), oxidation stone
Black alkene, Graphene, zinc oxide nano-particle, zinc oxide nanowire, zinc oxide nano rod, Nano silver grain, nano silver wire, gold
Any one in nanoparticle, boron nitride nanosheet, boron nitride nanometer line and CNT or two or more combinations, but do not limit
In this.
More preferred, described CNT includes the group of SWCN, any one or two kinds in multi-walled carbon nano-tubes
Close, but not limited to this.
In one more preferred embodiment, the preparation method of described carbon nano tube composite fibre specifically includes following steps:
From carbon nano-tube film can be pulled out spinning carbon nano pipe array, and described thin film one end is fixed on collection device；
Can the select location setting between spinning carbon nano pipe array and described collection device comprise to select the liquid phase body of material described
System, and be in flattened state when described carbon nano-tube film is at described select location；
Described carbon nano-tube film is made by from can pull straight in spinning carbon nano pipe array by described collection device, and in continuous warp
Cross and be fully contacted with described liquid-phase system during described select location, so that described selected material is sufficient filling with the described CNT of composition
Between the CNT of film and/or be attached to the carbon nano tube surface forming described carbon nano-tube film；
Collect and twist described carbon nano-tube film formation fiber simultaneously so that described collection device is continuous, thus obtaining described CNT
Composite fibre.
In a preferred embodiment, described preparation method also includes: described carbon nano tube composite fibre is dried and high temperature
Process.
More preferred, the condition of described high-temperature process includes: carries out high temperature in protective atmosphere (inert atmosphere such as such as argon)
Process, temperature is 100～1000 DEG C, the time is more than 1h.
The embodiment of the present invention additionally provides a kind of carbon nano tube composite fibre, and it comprises complex root CNT and assembles the threadiness being formed
Structure and be at least dispersed in selected material in described filamentary structure, the most of carbon nanometer in this complex root CNT
Pipe is wound around along the axially continuous spiral extension of described composite fibre and mutually.
Further, at least part of carbon nano tube surface in this complex root CNT is attached with described selected material.
Further, it is formed in the gap between CNT and described selected material is distributed with.
Further, described selected material selects organic substance and/or inorganic substances, preferably includes pyrene, poly- 3- hexyl thiophene, poly- pyrrole
Cough up, graphene oxide, Graphene, zinc oxide nano-particle, zinc oxide nanowire, zinc oxide nano rod, Nano silver grain, silver
Any one in nano wire, golden nanometer particle, boron nitride nanosheet, boron nitride nanometer line and CNT or two or more groups
Close, but not limited to this.
More preferred, described CNT includes the group of SWCN, any one or two kinds in multi-walled carbon nano-tubes
Close, but not limited to this.
Shown in Figure 1, it is the schematic flow sheet of the present invention one exemplary embodiments, a kind of carbon nano tube composite fibre therein
Preparation method comprises the steps:
A. providing can spinning carbon nano pipe array；
B. pull out carbon nano-tube film from array；
C., another complex liquid a is provided；
D. described carbon nano-tube film is pulled straight, make carbon nano-tube film rectangular area pass through complex liquid a, then collect into fibre
Dimension, obtains described carbon nano tube composite fibre；
E. described carbon nano tube composite fibre is dried, and makees high-temperature process, can get the more preferable carbon nano tube composite fibre of performance.
Wherein, different selected materials (compound substance), liquid-phase system (complex liquid) and different complex liquid concentration are selected,
The carbon nano tube composite fibre of different composite proportioning can be obtained.
Below in conjunction with drawings and Examples, the technology of the present invention is further explained.
Embodiment 1
(1) preparation of carbon nano tube/graphene composite fibre: take can spinning carbon nano pipe array a piece of, and scrape from this array
Carbon nano-tube film, draws after this thin film makes it be fixed on collection device with tweezers, by concentration about 0.1mg/ml～16mg/ml's
Graphene oxide (single or multiple lift) solution is placed in below carbon nano-tube film, makes carbon nano-tube film at the uniform velocity simultaneously by collection device
Stable is collected by graphene oxide solution and the process of twisting simultaneously again, obtains CNT/graphene oxide composite fibre.
(2) high-temperature process of carbon nano tube/graphene composite fibre: CNT/graphene oxide prepared by step (1) is multiple
Condensating fiber is put in tube furnace, in argon protection atmosphere, controls temperature to be incubated 4～5h under the conditions of 100～1000 DEG C, can obtain
Performance more preferable carbon nano tube/graphene composite fibre.
Shown in Figure 2, the present embodiment utilizes the carbon nano tube/graphene of the graphene oxide dispersion preparation of concentration about 3mg/ml
The tensile property of composite fibre is far superior to pure carbon nanotube fibers.
Embodiment 2
(1) preparation of carbon nano tube/silver Nanocomposites fiber: take can spinning carbon nano pipe array a piece of, scrape from this array
Go out carbon nano-tube film, drawn after this thin film makes it be fixed on collection device with tweezers, (solvent can be by silver nano-particle solution
The dispersible solvent of the Nano silver grains such as water, ethanol, Nano silver grain can be silver nanoparticle ball, multiple nanostructured such as nano silver wire)
It is placed in below carbon nano-tube film, make carbon nano-tube film at the uniform velocity and stable entering again by silver nano-particle solution by collection device
Row is collected and twisting simultaneously is processed, and obtains carbon nano tube/silver Nanocomposites fiber.
(2) high-temperature process of carbon nano tube/silver Nanocomposites fiber: carbon nano tube/silver nanoparticle prepared by step (1)
Sub- composite fibre is put in tube furnace, in argon protection atmosphere, controls temperature to be incubated about 5h under the conditions of 100～1000 DEG C, can
Obtain performance more preferable carbon nano tube/silver Nanocomposites fiber.
Referring to Fig. 3, the electric conductivity of the present embodiment carbon nano tube/silver Nanocomposites fiber is far superior to pure carbon nanotube fibers.
Comparative example
(1) preparation of post processing formula carbon nano tube/graphene composite fibre: take can spinning carbon nano pipe array a piece of, and from this battle array
Scrape carbon nano-tube film in row, drawn after this thin film makes it be fixed on collection device with tweezers, carbon nanometer is made by collection device
Pipe thin film at the uniform velocity and stable be collected and twisting simultaneously is processed, obtain carbon nano-tube fibre.Concentration is taken to be 0.01～16mg/ml
Graphene oxide dispersion Deca is in prepared carbon nano-tube fibre, and so that it is fully contacted, and obtains post processing formula CNT/stone
Black alkene composite fibre.
(2) high-temperature process of post processing formula carbon nano tube/graphene composite fibre: post processing formula carbon nanometer prepared by step (1)
Pipe/Graphene composite fibre is put in tube furnace, in argon protection atmosphere, controls temperature to be incubated under the conditions of 100～1000 DEG C
4～5h, availability more preferable post processing formula carbon nano tube/graphene composite fibre.
Shown in Figure 4, this comparative example utilizes the carbon nano tube/graphene of the graphene oxide dispersion preparation of concentration about 3mg/ml
The tensile property of composite fibre is slightly better than pure carbon nanotube fibers, and is much weaker than the like product that the embodiment of the present invention 1 is obtained.
Additionally, inventor is referring also to the scheme of previous embodiment 1-2, using the other raw materials addressed in this specification and technique
Condition, has been obtained other a series of carbon nano tube composite fibre products, and then also the performance of these products has been tested, its
Result is basically identical with embodiment 1-2.
It should be appreciated that above-described embodiment technology design only to illustrate the invention and feature, its object is to allow and be familiar with technique
Personage will appreciate that present disclosure and implements according to this, can not be limited the scope of the invention with this.All smart according to the present invention
Equivalence changes or modification that god's essence is made, all should be included within the scope of the present invention.
Claims (14)
1. a kind of preparation method of carbon nano tube composite fibre is it is characterised in that include: from continuously can drawing spinning carbon nano pipe array
Go out carbon nano-tube film, and make described carbon nano-tube film keep flattened state and continuously and stably with comprise to select the liquid phase body of material
System is fully contacted, so that described selected material is sufficient filling between the CNT of the described carbon nano-tube film of composition and/or is attached to group
Becoming the carbon nano tube surface of described carbon nano-tube film, receiving integrated fibers afterwards, thus obtaining described carbon nano tube composite fibre.
2. preparation method according to claim 1 is it is characterised in that include: makes described carbon nano-tube film keep flattened state
And continuously and stably passed through from described liquid-phase system with setting speed, receive integrated fibers afterwards.
3. preparation method according to claim 1 is it is characterised in that include: makes described carbon nano-tube film and described liquid phase
After system is fully contacted, regathers and twisting forms described fiber simultaneously.
4. preparation method according to claim 1 it is characterised in that: described liquid-phase system comprise solvent and be dissolved in and/or
It is dispersed in the selected material in described solvent.
5. preparation method according to claim 4 is it is characterised in that described solvent includes water and/or organic solvent, preferably
, described organic solvent includes ethanol, isopropanol, n, any one in n- dimethylformamide, dimethyl sulfoxide, chloroform etc.
Plant or two or more combinations.
6. the preparation method according to any one of claim 1 or 4 it is characterised in that: described selected material includes can be molten
In the material of described solvent and/or the material that can be dispersed in described solvent is it is preferred that described selected material includes aoxidizing stone
Black alkene, Graphene, zinc oxide nano-particle, zinc oxide nanowire, zinc oxide nano rod, Nano silver grain, nano silver wire, gold
Any one in nanoparticle, boron nitride nanosheet, boron nitride nanometer line and CNT or two or more combinations.
7. preparation method according to claim 1 it is characterised in that: described CNT includes SWCN, Duo Bi
The combination of any one or two kinds in CNT.
8. preparation method according to claim 1 is it is characterised in that include:
From carbon nano-tube film can be pulled out spinning carbon nano pipe array, and described thin film one end is fixed on collection device；
Can the select location setting between spinning carbon nano pipe array and described collection device comprise to select the liquid phase body of material described
System, and be in flattened state when described carbon nano-tube film is at described select location；
Described carbon nano-tube film is made by from can pull straight in spinning carbon nano pipe array by described collection device, and in continuous warp
Cross and be fully contacted with described liquid-phase system during described select location, so that described selected material is sufficient filling with the described CNT of composition
Between the CNT of film and/or be attached to the carbon nano tube surface forming described carbon nano-tube film；
Collect and twist described carbon nano-tube film formation fiber simultaneously so that described collection device is continuous, thus obtaining described CNT
Composite fibre.
9. the preparation method according to any one of claim 1-8 is it is characterised in that also include: described CNT is combined
Fiber is dried and high-temperature process.
10. preparation method according to claim 9 is it is characterised in that the condition of described high-temperature process includes: in protectiveness
Carry out high-temperature process, temperature is 100～1000 DEG C, the time is more than 1h in atmosphere.
A kind of 11. carbon nano tube composite fibres it is characterised in that comprise complex root CNT assemble formed filamentary structure and
At least it is dispersed in the selected material in described filamentary structure, the most of CNT in this complex root CNT is along described
The axially continuous spiral extension of composite fibre is simultaneously mutually wound around.
12. carbon nano tube composite fibres according to claim 11 it is characterised in that: in this complex root CNT at least
Part carbon nano tube surface is attached with described selected material；And/or, it is formed in the gap between CNT and described select is distributed with
Material.
13. preparation methoies according to claim 11 it is characterised in that: described selected material selects organic substance and/or no
Machine material, preferably includes conjugated molecule, graphene oxide, Graphene, zinc oxide nano-particle, zinc oxide nanowire, zinc oxide
In nanometer rods, Nano silver grain, nano silver wire, golden nanometer particle, boron nitride nanosheet, boron nitride nanometer line and CNT
Any one or two or more combinations.
14. preparation methoies according to claim 11 it is characterised in that: described CNT includes SWCN, many
The combination of any one or two kinds in wall carbon nano tube.
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Cited By (10)
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| CN107473203A (en) * | 2017-08-10 | 2017-12-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method and device of continuous producing carbon nano-tube laminated film or fiber |
| CN108070932A (en) * | 2017-12-18 | 2018-05-25 | 郑州大学 | A kind of preparation method for effectively improving single-walled carbon nanotube fibrous mechanical property |
| CN109563649A (en) * | 2017-02-03 | 2019-04-02 | 株式会社Lg化学 | The carbon nano-tube fibre for being used to prepare the method for carbon nano-tube fibre and thus preparing |
| RU2690821C1 (en) * | 2018-04-27 | 2019-06-05 | Автономная некоммерческая образовательная организация высшего образования Сколковский институт науки и технологий | Method of producing strong and current-conducting fiber by drawing films from carbon nanotubes |
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