CN109232980A - A kind of carbon nanotube and preparation method thereof - Google Patents

A kind of carbon nanotube and preparation method thereof Download PDF

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Publication number
CN109232980A
CN109232980A CN201810577528.3A CN201810577528A CN109232980A CN 109232980 A CN109232980 A CN 109232980A CN 201810577528 A CN201810577528 A CN 201810577528A CN 109232980 A CN109232980 A CN 109232980A
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carbon nanotube
carbon
carbon nano
solution
tube film
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关贵清
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Ningde Normal University
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Ningde Normal University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/041Carbon nanotubes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/08Ingredients agglomerated by treatment with a binding agent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Carbon nanotube of the present invention is made of the first carbon nanometer film, toughness material layer, the second carbon nano-tube film, graphene layer stacking;A kind of preparation method of carbon nanotube includes the following steps: S1, is put into carbon nano-tube film in the mixed solution of leavening agent, compatilizer and resin matrix;After the leavening agent in mixed solution penetrates into carbon nano-tube film inside, so that the structure of carbon nano-tube film is gradually loose, and enters resin matrix molecule inside carbon nano-tube film, preliminary carbon nano-tube material is formed;S2, it prepares dispersion liquid graphite is dissolved in solution, and dispersing agent is added, form dispersion liquid;Ultrasonic wave effect will be ultrasonic in dispersion liquid;The layering of laminar flow plasma is by dispersion liquid as the processing of laminar flow plasma beam;Dispersion liquid is carried out ultrasonic layering by molding again, obtains molding graphene layer;S3, the carbon nano-tube material preliminarily formed, toughness material layer, graphene layer successively through sinter molding and hot extrusion molding process, are obtained into carbon nanotube.

Description

A kind of carbon nanotube and preparation method thereof
Technical field
The present invention relates to technical field of nano material, specifically a kind of carbon nanotube and preparation method thereof.
Background technique
Carbon nanotube is as monodimension nanometer material, and light-weight, hexagonal structure connection is perfect, has many abnormal power , electricity and chemical property;Goed deep into its wide application prospect also not with carbon nanotube and nano materials research in recent years It shows disconnectedly;Carbon nanotube also known as Baji-tube are that a kind of have special construction (radial dimension is nanometer scale, axial ruler It is very little be micron dimension, pipe both ends are substantially all sealing) One-dimensional Quantum material.Carbon nanotube is mainly by hexagonal arrangement Carbon atom constitutes several layers to tens of layers of coaxial round tube.The distance being kept fixed between layers, about 0.34nm, diameter are generally 2~20nm.And zigzag, armchair and screw type three can be divided into along axial different orientation according to carbon hexagon Kind.Wherein the carbon nanotube of screw type has chirality, and zigzag and armchair carbon nanotubes are without chirality.
With going deep into for nano materials research, the wide application prospect of graphene and carbon nano tube compound material is also continuous Ground is shown, however, carbon nanotube in the prior art is first to receive graphene fragment and carbon with graphene composite film After mitron powder is scattered in solution, then by above-mentioned mixed liquor film forming made from, the above method obtain graphene and carbon nanometer In the composite construction of pipe, graphene is also not with the appearance of whole stratiform, since graphene is scattered in the form of a large amount of fragments In above-mentioned composite construction, so that the composite construction electric conductivity and toughness of above-mentioned graphene and carbon nanotube are also not strong enough, because This limits the application of graphene and carbon nano tube compound material.
Summary of the invention
The purpose of the present invention is to provide a kind of carbon nanotubes and preparation method thereof, to solve to propose in above-mentioned background technique The problem of.
To achieve the above object, the invention provides the following technical scheme:
A kind of carbon nanotube and preparation method thereof, the carbon nanotube is by the first carbon nanometer film, toughness material layer, second Carbon nano-tube film, graphene layer stacking composition;
A kind of preparation method of carbon nanotube, which comprises the steps of:
S1, carbon nano-tube film is put into the mixed solution of leavening agent, compatilizer and resin matrix;When in mixed solution After leavening agent penetrates into carbon nano-tube film inside, generation microbubble can be decomposed, micro-explosion effect is generated, so that the knot of carbon nano-tube film Structure is gradually loose, while playing the role of removal of impurities;And enter resin matrix molecule inside carbon nano-tube film, it forms preliminary carbon and receives Nanotube material;
S2, it prepares dispersion liquid graphite is dissolved in solution, and dispersing agent is added, form point that concentration is 0.02-0.06% Dispersion liquid;Ultrasonic wave is acted on ultrasound 40-95min in dispersion liquid;The layering of laminar flow plasma is by dispersion liquid as laminar flow plasma beam Handle 30-65min;Dispersion liquid is carried out ultrasonic layering by molding again, obtains molding graphene layer;
S3, by the carbon nano-tube material preliminarily formed, toughness material layer, graphene layer successively through sinter molding and hot extrusion Molding procedure obtains carbon nanotube.
Further, the toughness material layer by neoprene, nitrile rubber, carbon black, aluminium, processing aid, subtract aluminium oxide Agent, aluminium oxide, tributyl citrate, the formula composition of sulphur.
Further, in the step S1, the form of carbon nano-tube film be single-walled carbon nanotube, multi-walled carbon nanotube or The combination of single-walled carbon nanotube and multi-walled carbon nanotube;Carbon nano-tube film is the group of conductor, semiconductor or conductor and semiconductor It is fit.
Further, in the step S1, compatilizer is the solution to dissolve each other with carbon nano-tube film;Described and carbon nano-tube film The solution to dissolve each other is ethanol solution, acetone soln or dichloromethane solution.
Further, in the step S1, leavening agent is the hydrogenperoxide steam generator of mass percent concentration 10%~75%, Or the mixed liquor of the dilution heat of sulfuric acid of mass percent concentration 8% and metallic zinc powder;Or mass percent concentration 12% is dilute The mixed liquor of nitric acid solution and sodium sulfite.
Further, in the step S1, resin matrix is poly-vinyl alcohol solution or resin solution, or be dissolved in alcohol or The fluoropolymer resin of person's acetone;Or it is dissolved in the nano granule suspension of alcohol or acetone and the mixed liquor of resin matrix.
Further, solution is N-methyl pyrrolidones in the step S2.
Further, in the step S3, sinter molding process is formed using cold moudling or vacuum heating-press sintering.
Compared with prior art, the beneficial effects of the present invention are: the present invention can guarantee the structure of carbon nanotube in structure Intensity, toughness material layer are effectively improved the mechanical characteristic of the composite material, and graphene layer is compounded on the second carbon nano-tube film, protect Composite material safety when in use and practicability are demonstrate,proved, is conducive to set in microelectronic field, superconduction sciemtifec and technical sphere, computer For the application in field, the leavening agent in mixed solution proposed by the present invention has certain oxidation, aoxidizes carbon pipe surface The binding force with fluoropolymer resin is improved, the comprehensive performance for improving carbon nano tube compound material is conducive to.
Detailed description of the invention
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
Fig. 1 is schematic structural view of the invention.
It is as shown in the figure: the first carbon nano-tube film 1, toughness material layer 2, the second carbon nano-tube film 3, graphene layer 4.
Specific embodiment
A kind of carbon nanotube and preparation method thereof, the carbon nanotube is by the first carbon nanometer film, toughness material layer, second Carbon nano-tube film, graphene layer stacking composition;
A kind of preparation method of carbon nanotube, which comprises the steps of:
S1, carbon nano-tube film is put into the mixed solution of leavening agent, compatilizer and resin matrix;When in mixed solution After leavening agent penetrates into carbon nano-tube film inside, generation microbubble can be decomposed, micro-explosion effect is generated, so that the knot of carbon nano-tube film Structure is gradually loose, while playing the role of removal of impurities;And enter resin matrix molecule inside carbon nano-tube film, it forms preliminary carbon and receives Nanotube material;
S2, it prepares dispersion liquid graphite is dissolved in solution, and dispersing agent is added, form point that concentration is 0.02-0.06% Dispersion liquid;Ultrasonic wave is acted on ultrasound 40-95min in dispersion liquid;The layering of laminar flow plasma is by dispersion liquid as laminar flow plasma beam Handle 30-65min;Dispersion liquid is carried out ultrasonic layering by molding again, obtains molding graphene layer;
S3, by the carbon nano-tube material preliminarily formed, toughness material layer, graphene layer successively through sinter molding and hot extrusion Molding procedure obtains carbon nanotube.
Further, the toughness material layer by neoprene, nitrile rubber, carbon black, aluminium, processing aid, subtract aluminium oxide Agent, aluminium oxide, tributyl citrate, the formula composition of sulphur.
Further, in the step S1, the form of carbon nano-tube film be single-walled carbon nanotube, multi-walled carbon nanotube or The combination of single-walled carbon nanotube and multi-walled carbon nanotube;Carbon nano-tube film is the group of conductor, semiconductor or conductor and semiconductor It is fit.
Further, in the step S1, compatilizer is the solution to dissolve each other with carbon nano-tube film;Described and carbon nano-tube film The solution to dissolve each other is ethanol solution, acetone soln or dichloromethane solution.
Further, in the step S1, leavening agent is the hydrogenperoxide steam generator of mass percent concentration 10%~75%, Or the mixed liquor of the dilution heat of sulfuric acid of mass percent concentration 8% and metallic zinc powder;Or mass percent concentration 12% is dilute The mixed liquor of nitric acid solution and sodium sulfite;Compatilizer in mixed solution can dissolve each other with carbon nanotube, and leavening agent and carbon is made to receive Mitron film resin matrix enters inside carbon nano-tube film, provides premise for fluffy effect and the infiltration of resin;Leavening agent has one Fixed oxidation makes the oxidation of carbon pipe surface improve the binding force with fluoropolymer resin, is conducive to improve carbon nanotube composite The comprehensive performance of material.
Further, in the step S1, resin matrix is poly-vinyl alcohol solution or resin solution, or be dissolved in alcohol or The fluoropolymer resin of person's acetone;Or it is dissolved in the nano granule suspension of alcohol or acetone and the mixed liquor of resin matrix.
Further, solution is N-methyl pyrrolidones in the step S2.
Further, in the step S3, sinter molding process is formed using cold moudling or vacuum heating-press sintering.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, It is still possible to modify the technical solutions described in the foregoing embodiments, or part of technical characteristic is carried out etc. With replacement, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this Within the protection scope of invention.

Claims (8)

1. a kind of carbon nanotube and preparation method thereof, which is characterized in that the carbon nanotube is by the first carbon nanometer film, toughness material The bed of material, the second carbon nano-tube film, graphene layer stacking composition.
Include the following steps:
S1, carbon nano-tube film is put into the mixed solution of leavening agent, compatilizer and resin matrix;When bulk in mixed solution After carbon nano-tube film inside is penetrated into agent, generation microbubble can be decomposed, generate micro-explosion effect so that the structure of carbon nano-tube film by It is gradually loose, while playing the role of removal of impurities;And enter resin matrix molecule inside carbon nano-tube film, form preliminary carbon nanotube Material.
S2, it prepares dispersion liquid graphite is dissolved in solution, and dispersing agent is added, form the dispersion liquid that concentration is 0.02-0.06%; Ultrasonic wave is acted on ultrasound 40-95min in dispersion liquid;The layering of laminar flow plasma is by dispersion liquid as the processing of laminar flow plasma beam 30-65min;Dispersion liquid is carried out ultrasonic layering by molding again, obtains molding graphene layer.
S3, by the carbon nano-tube material preliminarily formed, toughness material layer, graphene layer successively through sinter molding and hot extrusion molding Process obtains carbon nanotube.
2. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that the toughness material layer is by chlorine Buna, carbon black, aluminium, processing aid, subtracts aluminium oxide agent, aluminium oxide, tributyl citrate, the formula group of sulphur at nitrile rubber At.
3. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that in the step S1, carbon is received The form of mitron film is the combination of single-walled carbon nanotube, multi-walled carbon nanotube or single-walled carbon nanotube and multi-walled carbon nanotube; Carbon nano-tube film is the assembly of conductor, semiconductor or conductor and semiconductor.
4. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that compatible in the step S1 Agent is the solution to dissolve each other with carbon nano-tube film;The solution to dissolve each other with carbon nano-tube film is ethanol solution, acetone soln or two Chloromethanes solution.
5. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that bulk in the step S1 Agent be mass percent concentration 10%~75% hydrogenperoxide steam generator or mass percent concentration 8% dilution heat of sulfuric acid with The mixed liquor of metallic zinc powder;Or mass percent concentration 12% dilute nitric acid solution and sodium sulfite mixed liquor.
6. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that in the step S1, resin Matrix is poly-vinyl alcohol solution or resin solution, or is dissolved in the fluoropolymer resin of alcohol or acetone;Or it is dissolved in alcohol or third The nano granule suspension of ketone and the mixed liquor of resin matrix.
7. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that solution is in the step S2 N-methyl pyrrolidones.
8. a kind of carbon nanotube as described in claim 1 and preparation method thereof, which is characterized in that in the step S3, sintering Molding procedure is formed using cold moudling or vacuum heating-press sintering.
CN201810577528.3A 2018-05-28 2018-05-28 A kind of carbon nanotube and preparation method thereof Pending CN109232980A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107828164A (en) * 2017-12-12 2018-03-23 东华大学 A kind of preparation method of carbon nano tube compound material
CN107841014A (en) * 2017-11-30 2018-03-27 李颂 A kind of toughness material formula
CN107879334A (en) * 2017-12-25 2018-04-06 成都锦汇科技有限公司 A kind of preparation method of graphene
CN207209967U (en) * 2017-09-05 2018-04-10 北京赛则科技有限公司 A kind of graphene composite structure of carbon nano tube

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN207209967U (en) * 2017-09-05 2018-04-10 北京赛则科技有限公司 A kind of graphene composite structure of carbon nano tube
CN107841014A (en) * 2017-11-30 2018-03-27 李颂 A kind of toughness material formula
CN107828164A (en) * 2017-12-12 2018-03-23 东华大学 A kind of preparation method of carbon nano tube compound material
CN107879334A (en) * 2017-12-25 2018-04-06 成都锦汇科技有限公司 A kind of preparation method of graphene

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Application publication date: 20190118