CN112900075B - SWNTs/MWNTs coaxial fiber and preparation method and application thereof - Google Patents
SWNTs/MWNTs coaxial fiber and preparation method and application thereof Download PDFInfo
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- 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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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- 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
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Abstract
The invention provides a SWNTs/MWNTs coaxial fiber and a preparation method and application thereof. The MWNTs coating layer and the SWNTs fiber are tightly connected through the amorphous carbon layer, the problem of direct growth and loading of the carbon nano tube as a substrate in the prior art is solved, the thickness of the MWNTs coating layer can reach 1-2 mm, micron-sized carbon nano tube fibers are increased to millimeter-sized, porous MWNTs are beneficial to filling of other polymers, such as resin and rubber compounding, and the SWNT/MWNT/polymer composite fiber with high tensile strength can be prepared.
Description
Technical Field
The invention relates to the technical field of nano material synthesis, in particular to SWNTs/MWNTs coaxial fiber and a preparation method and application thereof.
Background
Carbon nanotubes are considered to be one of the most strong materials currently found by man, having high young's modulus and tensile strength. However, the surface of carbon nanotubes has poor affinity and insufficient wettability, and is often not ideal for being compounded with high-strength polymer materials (such as resin and rubber). Generally, epoxy resin, polyvinyl alcohol and the like are commonly used as organic polymers of carbon nanotubes, but carbon nanotubes, especially fiber-type carbon nanotubes, have compact structures, and the loading amount of the polymers is often low. And the diameter of the carbon nanotube fiber is difficult to reach macroscopic millimeter size due to the limitation of the yield of the carbon nanotubes.
Disclosure of Invention
The invention provides a SWNTs/MWNTs coaxial fiber and a preparation method and application thereof, wherein a porous MWNTs coating layer is directly grown on the surface of the SWNTs fiber, the thickness of the MWNTs coating layer can reach 1-2 mm, so that micron-sized carbon nanotube fibers are increased to millimeter level, and the porous MWNTs are beneficial to filling of other polymers.
The technical scheme of the invention is realized as follows: the SWNTs/MWNTs coaxial fiber comprises single-walled carbon nanotube (SWNTs) fiber, wherein a coaxial multi-walled carbon nanotube (MWNTs) layer grows on the outer side of the SWNTs fiber, and the MWNTs coating layer is connected with the SWNTs fiber through an amorphous carbon layer.
Further, the MWNTs coating is the porous structure of the aerogel sponge.
A preparation method of SWNTs/MWNTs coaxial fibers comprises the following steps:
(1) Self-supporting and continuous SWNTs films prepared by chemical vapor deposition;
(2) Twisting and spinning a plurality of layers of SWNTs films to prepare SWNTs fibers;
(3) Suspending the SWNTs fiber into a tube furnace;
(4) And growing MWNTs coating layers on the surfaces of the SNWs fibers by adopting chemical vapor deposition.
Further, in the step (1), the SWNTs film is prepared by taking dimethylbenzene as a carbon source and ferrocene as a catalyst and is grown at 1200 ℃ in a hydrogen-argon mixed gas atmosphere.
Further, in the step (4), dichlorobenzene is used as a carbon source, ferrocene is used as a catalyst, and MWNTs grow in a hydrogen-argon mixed gas atmosphere at 860 ℃, so that the SWNTs/MWNTs coaxial fibers are obtained.
Further, in the step (3), two ends of the SWNTs fiber are respectively stuck to two sides of the quartz arc-shaped groove, so that the middle part of the SWNTs fiber is suspended, then another quartz arc-shaped groove is placed on the upper side of the quartz arc-shaped groove, and the two quartz arc-shaped grooves form a cylinder and are placed in the tube furnace.
An application of SWNTs/MWNTs coaxial fiber in a polymer reinforced material.
The SWNTs/MWNTs coaxial fiber is used in preparing SWNTs/MWNTs/polymer composite fiber.
The invention has the beneficial effects that:
the MWNTs coating layer is directly grown on the surface of the SWNTs fiber, the MWNTs coating layer is tightly connected with the SWNTs fiber through the amorphous carbon layer, the problem that the existing MWNTs coating layer is directly grown and loaded by taking the carbon nano tube as a substrate is solved, the MWNTs coating layer is composed of the porous multi-wall carbon nano tube, and the thickness of the MWNTs coating layer can reach 1-2 mm. The porous MWNTs coating layer enables micron-sized carbon nanotube fibers to be increased to a millimeter level, the porous MWNTs are beneficial to filling of other polymers, and the SWNT @ MWNT fibers are compounded with high-strength organic polymer materials such as resin and rubber, so that the SWNT/MWNT/polymer composite fibers with high tensile strength can be prepared.
Compared with other fibers such as carbon fibers, the SWNTs fiber adopted by the invention has the following advantages: (1) Carbon nanotube fibers and carbon fibers are essentially two substances of carbon, and both have excellent mechanical strength, but the carbon nanotube fibers have more excellent flexibility, and can be subjected to deformation treatment such as patterning, weaving or spiral treatment in the preparation process, so that composite materials with more complex structures can be prepared, for example, SWNTs fibers have smaller curvature radius and can be subjected to more extreme deformation, and different internal stress and shaft diameter requirements are provided, for example: by further twisting the motor, a helical structure may be formed; (2) The diameter of the carbon nano tube fiber is controllable, and the SWNTs/MWNTs coaxial fiber with different diameter ratios can be prepared by controlling the thickness of the film before spinning; (3) The SWNTs @ MWNTs coaxial fiber solves the problem of poor interface bonding in the surface compounding process of the carbon nanotube fiber, the core-shell of the SWNTs/MWNTs coaxial fiber is tightly combined through the amorphous carbon layer, the outer sponge provides a support for the composite polymer, and the polymer is tightly combined with the amorphous carbon layer.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural view of a SWNTs/MWNTs coaxial fiber of the present invention;
FIG. 2 is a scanning electron micrograph of SWNTs/MWNTs coaxial fibers;
FIG. 3 is a scanning electron micrograph of the MWNTs coating layer;
FIG. 4 is a scanning electron micrograph of SWNTs/MWNTs/epoxy composite fibers;
FIG. 5 is a stress-strain curve of SWNTs/MWNTs coaxial fibers and SWNTs/MWNTs/epoxy composite fibers;
FIG. 6 is a scanning electron micrograph of the helical structure of SWNTs fibers.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without inventive step, are within the scope of the present invention.
A SWNTs/MWNTs coaxial fiber comprises a SWNTs fiber 1, a MWNTs coating layer 5 which is coaxial with the SWNTs fiber 1 grows on the outer side of the SWNTs fiber 1, and the MWNTs coating layer 5 is connected with the SWNTs fiber 1 through an amorphous carbon layer 4. The MWNTs coating 5 is the porous structure of the aerogel sponge.
The preparation method of the SWNTs/MWNTs coaxial fiber comprises the following steps:
(1) Self-supporting and continuous SWNTs films prepared by chemical vapor deposition;
(2) Twisting and spinning a plurality of layers of SWNTs films to prepare SWNTs fibers;
(3) Suspending the SWNTs fiber into a tube furnace;
(4) And growing MWNTs coating layers on the surfaces of the SNWs fibers by adopting chemical vapor deposition.
In the step (1), the SWNTs film is prepared by taking dimethylbenzene as a carbon source and ferrocene as a catalyst and is grown at 1200 ℃ in a hydrogen-argon mixed gas atmosphere.
In the step (2), the diameter of the SWNTs fiber can be controlled by the layer number of the SWNTs film in the spinning process of the SWNTs film. The specific method of twist spinning is as follows: and overlapping a plurality of layers of the SWNTs films, fixing one end of the overlapped SWNTs films with a motor, fixing the other end of the overlapped SWNTs films with a weight, and starting the motor to drive the SWNTs films to rotate and weave the SWNTs films into cylindrical SWNTs fibers. The weight mass adopted by the invention is 100g.
In the step (3), two ends of the SWNTs fiber 1 are respectively adhered to two sides of the quartz arc-shaped groove 2, so that the middle part of the SWNTs fiber 1 is suspended, then another quartz arc-shaped groove is arranged on the upper side of the quartz arc-shaped groove 2, the two quartz arc-shaped grooves form a cylinder and are arranged in the tube furnace, and the outer diameters of the two quartz arc-shaped grooves are close to the inner diameter of the tube furnace.
In the step (4), dichlorobenzene is used as a carbon source, ferrocene is used as a catalyst, and MWNTs grow at 860 ℃ in the atmosphere of hydrogen and argon mixed gas to obtain the SWNTs/MWNTs coaxial fiber. The diameter of the SWNTs/MWNTs coaxial fibers can be controlled by the reaction time of step (4). In the step (4), firstly, the amorphous carbon layer is coated on the outer side of the SWNTs, and then MWNTs are grown on the amorphous carbon layer to form a MWNTs coating layer with the thickness of millimeters.
The following detailed description is given with reference to specific examples.
The method comprises the steps of taking dimethylbenzene as a carbon source and ferrocene as a catalyst, preparing a SWNTs film growing at 1200 ℃ in an argon-hydrogen (6).
With the SWNTs fibers having a smaller radius of curvature than the carbon fibers, a helical structure may be formed by further twisting the fibers with a motor, as shown in fig. 6.
The schematic structure of SWNTs/MWNTs coaxial fiber is shown in FIG. 1, with SWNTs fiber 1 as the axis, amorphous carbon layer as the adhesive layer, and porous MWNTs coating layer as the outer layer.
In order to characterize the microstructure of the SWNTs/MWNTs coaxial fiber, we performed scanning electron microscope characterization on the SWNTs/MWNTs coaxial fiber obtained in example 1, the port of the SWNTs/MWNTs coaxial fiber is shown in fig. 2 and 3, the SWNTs fiber is used as the shaft, the diameter is about 20 microns, the outer layer has a thin amorphous carbon layer, the SWNTs and the MWNTs are tightly connected, the thickness is about 5 microns, and the outermost layer has a porous MWNTs coating layer, the diameter can reach 1 mm.
Example 2
The SWNTs/MWNTs coaxial fiber has excellent conductivity and mechanical strength, and can be compounded with other high-strength polymers, such as resin and rubber to prepare the SWNT/MWNT/polymer composite fiber with high tensile strength. Putting the SWNTs/MWNTs coaxial fibers prepared in the example 1 into an epoxy resin solution, wherein the mass ratio of E-44 to E-31 in the epoxy resin (epoxy) solution is 25: and 10, after vacuum treatment, putting the composite fiber into a drying oven, and curing for 1 hour at 120 ℃ to obtain the SWNTs/MWNTs/epoxy resin composite fiber.
A scanning electron microscope of a port of the SWNTs/MWNTs/epoxy resin composite fiber is shown in figure 4, the SWNTs/MWNTs coaxial fibers are uniformly distributed in the polymer, the SWNTs/MWNTs coaxial fibers are closely related to the porous structure of MWNTs, and the porosity of the MWNTs is favorable for filling the polymer. At the fracture of the SWNTs/MWNTs/epoxy resin composite fiber, a large number of carbon nanotubes are exposed due to the high strength and high modulus of the carbon nanotubes, and the mechanical property of the SWNTs/MWNTs/epoxy resin composite material is enhanced in an epoxy matrix by the disordered and uniformly distributed carbon nanotubes.
The SWNTs/MWNTs coaxial fibers and the SWNTs/MWNTs/epoxy composite fibers prepared in examples 1 and 2 were subjected to a stretch-breaking test on a stretcher. The stress strain is shown in FIG. 5, the stress of the loaded SWNTs/MWNTs/epoxy resin composite fiber is about 55MPa, which is much higher than that of the SWNTs/MWNTs coaxial fiber (4 MPa), and simultaneously higher than that of the pure epoxy resin prepared by the same method (45 MPa).
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of SWNTs/MWNTs coaxial fibers is characterized by comprising the following steps:
(1) Self-supporting and continuous SWNTs films prepared by chemical vapor deposition;
(2) Twisting and spinning a plurality of layers of SWNTs films to prepare SWNTs fibers;
(3) Suspending the SWNTs fiber into a tube furnace;
(4) Adopting chemical vapor deposition to grow an MWNTs coating layer on the surface of the SNWTs fiber;
the SWNTs/MWNTs coaxial fiber comprises a SWNTs fiber, wherein a coaxial MWNTs coating layer grows on the outer side of the SWNTs fiber, the MWNTs coating layer is connected with the SWNTs fiber through an amorphous carbon layer, and the MWNTs coating layer enables the SWNTs/MWNTs coaxial fiber to reach a millimeter level;
in the step (4), dichlorobenzene is used as a carbon source, ferrocene is used as a catalyst, and MWNTs grow at 860 ℃ in the atmosphere of hydrogen and argon mixed gas to obtain the SWNTs/MWNTs coaxial fiber.
2. The method for preparing SWNTs/MWNTs coaxial fiber according to claim 1, wherein: the MWNTs coating layer is a porous structure of the aerogel sponge.
3. The method for preparing SWNTs/MWNTs coaxial fibers according to claim 1, wherein in the step (1), a SWNTs film is grown at 1200 ℃ in a hydrogen-argon mixed gas atmosphere by using xylene as a carbon source and ferrocene as a catalyst.
4. The method according to claim 1, wherein in the step (3), the two ends of the SWNTs fiber are respectively adhered to the two sides of the quartz arc-shaped groove, so that the middle part of the SWNTs fiber is suspended, then another quartz arc-shaped groove is arranged on the upper side of the quartz arc-shaped groove, and the two quartz arc-shaped grooves form a cylinder and are arranged in the tube furnace.
5. SWNTs/MWNTs coaxial fibres produced by the process of any one of claims 1 to 4.
6. Use of SWNTs/MWNTs coaxial fibres according to claim 5 in polymer reinforcement.
7. The SWNTs/MWNTs coaxial fiber of claim 5 used to prepare SWNTs/MWNTs/polymer composite fiber.
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| US7727504B2 (en) * | 2004-12-01 | 2010-06-01 | William Marsh Rice University | Fibers comprised of epitaxially grown single-wall carbon nanotubes, and a method for added catalyst and continuous growth at the tip |
| US20060177659A1 (en) * | 2005-02-09 | 2006-08-10 | National Pingtung University Of Science & Technology | Powder containing carbon nanotube or carbon nanofiber and process for preparing the same |
| WO2012019819A1 (en) * | 2010-08-13 | 2012-02-16 | Huntsman Advanced Materials (Switzerland) Gmbh | Process to grow carbon nanotubes onto fibers |
| CN104085873B (en) * | 2014-06-03 | 2016-11-02 | 张映波 | A kind of method preparing CNT in fiber surface high density |
| CN107541809B (en) * | 2016-06-24 | 2020-05-22 | 郑州大学 | Preparation method of high-strength, high-toughness and high-conductivity single-walled carbon nanotube fiber |
| CN109797540B (en) * | 2018-12-26 | 2020-10-30 | 山东大学 | Preparation method for carbon nanotube on-line continuous growth on carbon fiber surface |
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