TWI422524B - Method for making carbon nanotube composite - Google Patents

Description

Method for preparing nano carbon tube composite material

The invention relates to a preparation method of a composite material, in particular to a preparation method of a carbon nanotube composite material.

Since the discovery of Carbon Nanotube (CNT) by Iijima of NEC Corporation in Japan in 1991 (see Helical microtubules of graphitic carbon, Nature, Sumio Iijima, vol 354, p56 (1991)), carbon nanotubes have caused science. The great attention of the industry and the industry is a hot topic in international scientific research in recent years. The carbon nanotubes have the same thermal conductivity and unique mechanical properties as diamond, such as tensile strength up to 100 gigapascals, modulus up to 1800 gigapascals, resistance to strong acids and alkalis, and basic non-oxidation below 600 °C.

Due to the excellent performance of carbon nanotubes, the use of carbon nanotubes as fillers in combination with other materials has become an important direction for carbon nanotube applications. In particular, the combination of carbon nanotubes with other materials, such as metals, semiconductors or polymer materials, can complement or enhance the advantages of the materials. The carbon nanotube has a large aspect ratio and a hollow structure, and has excellent mechanical properties, and can be used as a super fiber to enhance the composite material. In addition, the carbon nanotubes have excellent thermal conductivity, and the thermal conductivity of the carbon nanotubes makes the composite have good thermal conductivity.

In the prior art, the carbon nanotube composite material is prepared in the form of a particle-filled polymer material. Since the carbon nanotube is easily agglomerated, the surface modification and functionalization of the carbon nanotube must be performed first, followed by solution or melting. square The method is compounded with a polymer material. A method for preparing a carbon nanotube composite material in the prior art includes the following steps: (1) 0.3 part by weight of the multi-walled carbon nanotube powder is put into 10 parts by weight of concentrated nitric acid, and stirred under reflux at 100 ° C for 20 hours. The acid solution was washed with distilled water and dried under vacuum at 90 ° C for 10 hours. (2) The above product carboxylated carbon nanotubes were added to 10 parts by weight of chlorophyll chloride, stirred at 90 ° C for 10 hours, and the unreacted was distilled off. The grass is chlorinated to obtain a ruthenium chloride carbon nanotube; (3) the ruthenium chlorided carbon nanotube is placed in an ice bath and stirred slowly, and 10 parts by weight of dry ethylenediamine is added dropwise at 100 Vacuum drying at °C for 10 hours; (4) Adding the above guanamined carbon nanotubes to 20 parts by weight of ethanol solvent, sonicating for 15 minutes, adding 2 parts by weight of epoxy resin, stirring at high speed for 20 minutes, steaming In addition to the solvent, the mixture is heated to 60 ° C, and the curing agent phenylenediamine is added in a ratio of 1:1 of the epoxy group of the epoxy resin to the amine hydrogen atom in the curing agent to uniformly disperse the carbon nanotubes; (5) Pour the composite system into the mold, heat it to 80 ° C and cure for 2 hours, then at 1 Curing at 50 ° C for 2 hours gave a carbon nanotube/epoxy composite.

The preparation method of the above carbon nanotube/epoxy composite material has the following disadvantages: First, in the preparation process of the carbon nanotube composite material, in order to better disperse the carbon nanotube in the polymer material, The carbon nanotube powder needs to be mixed with the polymer material and the surface modification of the carbon nanotubes, which will seriously damage the structure of the carbon nanotubes, thereby affecting the performance of the carbon nanotube composite; Second, in the process of preparing the carbon nanotube composite material, it is necessary to add a solvent, and the added solvent is difficult to remove, so that the composition of the carbon nanotube composite material is impure; thirdly, the method cannot realize the carbon nanotube composite in the composite Fixed orientation in the material, making the nano The carbon tube cannot exert its axial advantage in the composite material, thereby affecting the performance of the carbon nanotube composite material. Fourth, the preparation method of the carbon nanotube composite material requires surface modification of the carbon nanotube tube. It is dispersed by adding a solvent, and the process is complicated and the cost is high.

In view of this, it is necessary to provide a method for preparing a carbon nanotube composite material having excellent characteristics, and the preparation method is simple, easy to implement, and low in cost.

A method for preparing a carbon nanotube composite material, comprising the steps of: preparing a self-supporting carbon nanotube film structure; providing a liquid thermosetting polymer material; and impregnating the nanocarbon with the liquid thermosetting polymer material The film structure of the tube; curing the carbon nanotube film structure infiltrated by the liquid thermosetting polymer material to obtain a carbon nanotube composite material.

Compared with the prior art, the technical solution adopts a stretching tool to directly pull a carbon nanotube film from the carbon nanotube array, and the carbon nanotube film in the carbon nanotube film is uniformly distributed and arranged in a preferred orientation. Therefore, the preparation method of the carbon nanotube composite material has the following advantages: First, the carbon nanotube film uniformly distributed by the carbon nanotubes is combined with the liquid thermosetting polymer material, and the surface modification of the carbon nanotubes is not required, It will destroy the structure of the carbon nanotubes and improve the performance of the prepared carbon nanotube composites. Second, the preparation of the carbon nanotube composites without the use of additives during the preparation of the carbon nanotube film. It is relatively pure and has good performance. Thirdly, the carbon nanotube composite material is prepared by infiltrating the carbon nanotube film structure with the liquid thermosetting polymer material, which simplifies the preparation process and reduces the production cost.

The technical solution will be further described in detail below with reference to the accompanying drawings.

Referring to FIG. 1 , an embodiment of the present technical solution provides a method for preparing a carbon nanotube composite material 10 , which specifically includes the following steps:

Step 1: Prepare a self-supporting carbon nanotube film structure 12.

The preparation method of the self-supporting carbon nanotube film structure 12 specifically includes the following steps:

(1) Providing an array of carbon nanotubes, preferably the array is a super-sequential carbon nanotube array.

In this embodiment, the method for preparing the super-sequential carbon nanotube array adopts a chemical vapor deposition method, and the specific steps include: (a) providing a flat substrate, the substrate may be selected from a P-type or N-type germanium substrate, or selected The tantalum substrate is formed with an oxide layer. In this embodiment, a 4-inch tantalum substrate is preferably used; (b) a catalyst layer is uniformly formed on the surface of the substrate, and the catalyst layer material may be iron (Fe), cobalt (Co) or nickel ( Ni) or one of alloys of any combination thereof; (c) annealing the substrate on which the catalyst layer is formed in air at 700 ° C to 900 ° C for about 30 minutes to 90 minutes; (d) placing the treated substrate in the reaction In the furnace, it is heated to 500 ° C ~ 740 ° C in a protective gas atmosphere, and then reacted with a carbon source gas for about 5 minutes to 30 minutes to grow a super-aligned carbon nanotube array having a height of 200 μm to 400 μm. The super-sequential carbon nanotube array is a plurality of pure carbon nanotube arrays formed of carbon nanotubes that are parallel to each other and perpendicular to the substrate. The super-sequential carbon nanotube array contains substantially no impurities such as amorphous carbon or residual catalyst metal particles, etc., by controlling the growth conditions described above. Nano in the carbon nanotube array The carbon tubes are in close contact with each other to form an array by van der Waals forces. The area of the carbon nanotube array is substantially the same as the area of the substrate described above.

In this embodiment, the carbon source gas may be a chemically active hydrocarbon such as acetylene, ethylene or methane. The preferred carbon source gas in this embodiment is acetylene; the shielding gas is nitrogen or an inert gas, and the preferred shielding gas in this embodiment. It is argon.

It can be understood that the carbon nanotube array provided by the embodiment is not limited to the above preparation method. It can also be a graphite electrode constant current arc discharge deposition method, a laser evaporation deposition method, or the like.

(2) A carbon nanotube film is obtained by drawing from the above carbon nanotube array.

The process of extracting a carbon nanotube film from the carbon nanotube array comprises the following steps: (a) selecting a plurality of carbon nanotube bundle segments of a certain width from the carbon nanotube array, the technical solution is implemented. Preferably, the tape is contacted with a tape having a width to select a plurality of carbon nanotube bundle segments of a certain width; (b) the plurality of carbon nanotube bundle segments are stretched at a constant speed along a direction substantially perpendicular to the growth direction of the carbon nanotube array. The carbon nanotube bundle segment obtains a continuous carbon nanotube film in which the arrangement of the carbon nanotubes is parallel to the direction of stretching.

During the above stretching process, the plurality of carbon nanotube bundle segments are gradually separated from the substrate in the stretching direction under the action of the tensile force, and the selected plurality of carbon nanotube bundle segments are respectively associated with the other naphthalenes due to the van der Waals force. The carbon nanotube segments are continuously pulled out end to end to form a carbon nanotube film.

In the embodiment of the technical solution, since the CVD method is used on the 4-inch base The long super-sequential carbon nanotube array is further processed to obtain a carbon nanotube film, so the carbon nanotube film has a width of 0.01 cm to 10 cm and a thickness of 10 nm to 100 μm. The carbon nanotubes in the above carbon nanotube film are single-walled carbon nanotubes, double-walled carbon nanotubes or multi-walled carbon nanotubes. When the carbon nanotube in the carbon nanotube film is a single-walled carbon nanotube, the single-walled carbon nanotube has a diameter of 0.5 nm to 50 nm. When the carbon nanotubes in the carbon nanotube film are double-walled carbon nanotubes, the double-walled carbon nanotubes have a diameter of 1.0 nm to 50 nm. When the carbon nanotubes in the carbon nanotube film are multi-walled carbon nanotubes, the diameter of the multi-walled carbon nanotubes is from 1.5 nm to 50 nm.

Further, at least two carbon nanotube films are laid in parallel and without gaps to obtain a carbon nanotube layer, and at least two carbon nanotube layers are overlapped to form a carbon nanotube film structure 12. It can be understood that the carbon nanotube film structure 12 can also be obtained by overlapping at least two carbon nanotube films.

The carbon nanotube film structure 12 comprises a carbon nanotube layer or at least two overlapping carbon nanotube layers, and the adjacent two carbon nanotube layers are tightly bonded by van der Waals force. The carbon nanotube layer comprises a carbon nanotube film or at least two parallel and gap-free carbon nanotube films. The carbon nanotube film comprises a plurality of carbon nanotube bundles arranged end to end and arranged in a preferred orientation. The lengths of the carbon nanotube bundles in the carbon nanotube film are substantially the same, and the nanotube bundles are closely connected by van der Waals force. The carbon nanotube bundle includes a plurality of carbon nanotubes of equal length and arranged in parallel with each other, and the carbon nanotubes are closely connected by a van der Waals force. The carbon nanotubes in the at least two overlapping carbon nanotube layers are arranged in a preferred orientation in the same direction, and between the adjacent carbon nanotubes in the two carbon nanotube layers It has a cross angle α, 0 degree ≦α≦90 degrees, which can be prepared according to actual needs.

Further, the above-mentioned carbon nanotube film structure 12 may be used as it is, or may be used after being treated with an organic solvent. The process of treating the carbon nanotube film structure 12 with an organic solvent comprises: dropping an organic solvent onto the surface of the carbon nanotube film structure 12 by a test tube to infiltrate the entire carbon nanotube film structure 12, or the entire carbon nanotube tube The film structure 12 is immersed in a container containing an organic solvent to infiltrate. The organic solvent is a volatile organic solvent such as a mixture of one or more of ethanol, methanol, acetone, dichloroethane and chloroform, and ethanol is used in the embodiment of the present invention. After the carbon nanotube film structure 12 is infiltrated by an organic solvent, the parallel carbon nanotube segments in the carbon nanotube film are partially aggregated into the carbon nanotube bundle under the surface tension of the volatile organic solvent. . Therefore, the carbon nanotube film structure 12 has a small surface volume ratio, is non-tacky, and has good mechanical strength and toughness.

Referring to FIG. 2, a preferred carbon nanotube film structure 12 of the embodiment of the present invention includes a first carbon nanotube layer 121, a second carbon nanotube layer 122, a third carbon nanotube layer 123, and A fourth carbon nanotube layer 124. The first carbon nanotube layer 121, the second carbon nanotube layer 122, the third carbon nanotube layer 123 and the fourth carbon nanotube layer 124 are overlapped, and each nanocarbon layer The carbon nanotubes are arranged in a preferred orientation along a fixed direction. The arrangement direction of the carbon nanotubes in the adjacent two carbon nanotube layers is 90 degrees, and a plurality of microporous structures are formed, and the diameter of the micropores is 1 nm to 0.5 μm. The preparation method of the carbon nanotube film structure 12 includes: firstly, a first carbon nanotube layer 121 and a second carbon nanotube are prepared by the method in the first step. a layer 122, a third carbon nanotube layer 123 and a fourth carbon nanotube layer 124; secondly, the first carbon nanotube layer 121, the second carbon nanotube layer 122, the third nanocarbon The tube layer 123 and the fourth carbon nanotube layer 124 are disposed to overlap each other such that the arrangement of the carbon nanotubes in the second carbon nanotube layer 122 is different from the first carbon nanotube layer 121 and the third carbon nanotube layer 123. The alignment direction of the carbon nanotubes is 90 degrees, the arrangement direction of the carbon nanotubes in the third carbon nanotube layer 123 and the nano carbon in the second carbon nanotube layer 122 and the fourth carbon nanotube layer 124 The arrangement of the tubes is 90 degrees.

Step 2: providing a liquid thermosetting polymer material 14.

The method for preparing the liquid thermosetting polymer material 14 comprises the following steps: first, placing a polymer material in a container, heating the polymer material at not higher than 300 ° C, and stirring the polymer material. , the polymer material is uniformly mixed, and the stirring time is determined by the type and quality of the polymer material; secondly, an additive or a mixture of a plurality of additives is added to the uniformly stirred polymer material. a chemical reaction; then, heating the polymer material mixed with the additive at not higher than 300 ° C, and stirring the polymer mixed with the additive to uniformly mix the polymer material and the additive The stirring time is determined by the type and quality of the polymer material and the additive, thereby obtaining a liquid thermosetting polymer material 14.

The liquid thermosetting polymer material 14 has a viscosity of less than 5 Pa. Seconds, and can maintain this viscosity for more than 30 minutes at room temperature. It can be understood that if the thermosetting polymer material 14 is in a solid state at room temperature, the thermosetting polymer material 14 is first heated to be converted into a liquid thermosetting polymer material 14.

The thermosetting polymer material 14 includes an additive such as a polymer material and a curing agent, a modifier, a filler, or a diluent. The content of the polymer material accounts for 70% to 95% of the mass of the thermosetting polymer material, and the content of the additive accounts for 5% to 30% of the mass of the thermosetting polymer material.

The polymer material is phenolic resin, epoxy resin, bismaleimide resin, polybenzoxazine resin, cyanate resin, polyimine resin, polyurethane, polymethyl methacrylate and unsaturated One or a mixture of polyfluorene resins and the like.

The curing agent is used to promote curing of the thermosetting polymer material 14. Commonly used curing agents include one or a mixture of a fatty amine, an alicyclic amine, an aromatic amine, a polyamine, an acid anhydride, a resin, and a tertiary amine. The modifier is used to improve the flexibility, shear resistance, bending resistance, impact resistance or insulation of the thermosetting polymer material 14. Commonly used modifiers include one or a mixture of polysulfide rubber, polyamide resin, polyvinyl butyral or nitrile rubber. The filler is used to improve heat dissipation conditions when the thermosetting polymer material 14 is cured, and the filler can also reduce the amount of the thermosetting polymer material and reduce the cost. Commonly used fillers include one or a mixture of asbestos fiber, glass fiber, quartz powder, porcelain powder, alumina and tannin powder. The diluent serves to lower the viscosity of the resin and improve the permeability of the resin. The diluent includes diglycidyl ether, polyglycidyl ether, propylene oxide butyl ether, propylene oxide phenyl ether, dipropylene oxide ethyl ether, tripropylene oxide propyl ether and allyl phenol. One or several mixes.

The embodiment of the technical solution preferably prepares the liquid thermosetting polymer material 14 by using an epoxy resin, which specifically includes the following steps: First, the glycidyl ether A mixture of epoxy and glycidyl ester epoxy is placed in a container, heated to 30 ° C to 60 ° C, and the mixture of the glycidyl ether epoxy and glycidyl ester epoxy in the container is stirred for 10 minutes. Until the mixture of the glycidyl ether type epoxy and the glycidyl ester type epoxy is uniformly mixed; secondly, the fatty amine and diglycidyl ether are added to the uniformly stirred glycidyl ether type epoxy and glycidyl ester a chemical reaction is carried out in a mixture of epoxy groups; finally, a mixture of the glycidyl ether epoxy and glycidyl ester epoxy is heated to 30 ° C to 60 ° C to obtain a liquid thermosetting polymer containing epoxy resin. Material 14. The epoxy-containing liquid thermosetting polymer material 14 is a liquid which is uniformly mixed in a transparent pale yellow color.

Step 3: The liquid thermosetting polymer material 14 is impregnated into the carbon nanotube film structure 12.

As shown in FIG. 3, step three can be implemented in a molding apparatus 100. The molding apparatus 100 includes a material supply device 20, a material input device 30, a mold 40, and a material output device 50. The raw material supply device 20 includes a container 201 for holding a raw material; the container 201 has an inlet 202 and a pressurizing port 203 for evacuating the container 201, the pressurizing The port 203 is for applying an injection pressure to the raw material in the container 201. The material input device 30 includes a valve 301 for controlling the inflow of the raw material, and an injection port 302 for injecting the raw material into the mold 40. The mold 40 has an upper mold 401 and a lower mold 402. The surface of the upper mold 401 and the lower mold 402 is evenly coated with a release agent so that the composite material can be smoothly released after obtaining the composite material. The release agent varies depending on the type of thermosetting polymer material. The release agent can be High temperature release agent, organic oxime release agent, wax release agent or siloxane type release agent. The material output device 50 includes a valve 501 for controlling the outflow of the raw material, and an outlet 502 for discharging the raw material out of the molding apparatus 100.

The method for infiltrating the liquid thermosetting polymer material 14 into the carbon nanotube film structure 12 in the embodiment of the technical solution comprises the following steps:

(1) A carbon nanotube film structure 12 is placed in a mold 40.

Applying a release agent to the surface of the upper mold 401 and the lower mold 402 in the mold 40, and placing the carbon nanotube film structure 12 in the cavity of the lower mold 402 of the mold 40, The mold 401 is gently placed over the lower mold 402. At the same time, the mold 40 is sealed using a gasket or sealant.

(2) The liquid thermosetting polymer material 14 is placed in a container 201, and the container 201 is evacuated, and an injection pressure is applied to the liquid thermosetting polymer material 14.

The valve 301 in the raw material input device 30 and the valve 501 in the raw material output device 50 are closed. The thermosetting polymer material 14 is placed in the container 201 of the material supply device 20. The container 201 is evacuated through the inlet 202 of the raw material supply device 20 to a vacuum of less than -0.09 MPa, and maintained at the vacuum for at least 10 minutes to sufficiently eliminate the introduction into the The air in the thermoset material 14. Next, an injection pressure is applied to the thermosetting polymer material 14 in the container 201 through the pressurizing port 203 of the material supply device 20. The applied injection pressure is measured in the range of 0.001 MPa to 10 MPa.

(3) The liquid thermosetting polymer material 14 is injected into the mold 40 to infiltrate the carbon nanotube film structure 12.

The valve 301 of the raw material input device 30 and the valve 501 of the raw material output device 50 are opened. The thermosetting polymer material 14 enters the mold 40 from the container 201 through the raw material input device 30 under the action of injection pressure, and infiltrates the carbon nanotube film structure 12.

The viscosity of the liquid thermosetting polymer material 14 is very low, and the carbon nanotube film structure 12 has a preferred orientation of the carbon nanotubes, and the adjacent carbon nanotubes have a certain gap therebetween, so the liquid thermosetting property is high. The molecular material 14 is well infiltrated into the gap formed between the carbon nanotubes. Therefore, the carbon nanotube composite material 10 has excellent properties. In order for the liquid thermosetting polymer material 14 to sufficiently wet the carbon nanotube film structure 12, the carbon nanotube film structure 12 may be infiltrated for not less than 10 minutes. At the same time, the excess liquid thermosetting polymer material 14 flows out through the outlet 502 of the material output device 50. The flowing thermosetting polymer material 14 carries out the air in the gap between the carbon nanotubes in the carbon nanotube film structure 12, and completely excludes the air in the carbon nanotube composite material 10, thereby not causing the naphthalene The carbon nanotube composite material 10 has structural defects.

It can be understood that the method of infiltrating the liquid thermosetting polymer material 14 into the carbon nanotube film structure 12 is not limited to an injection method, and the liquid thermosetting polymer material 14 can also be sucked into the nanometer by capillary action. In the carbon nanotube film structure 12, the carbon nanotube film structure 12 is impregnated, or the carbon nanotube film structure 12 is immersed in the liquid thermosetting polymer material 14.

Step 4: curing the carbon nanotube film structure 12 infiltrated by the liquid thermosetting polymer material 14 to obtain a carbon nanotube composite material 10.

The method for curing the carbon nanotube film structure 12 infiltrated by the liquid thermosetting polymer material 14 in the embodiment of the present technical solution comprises the following steps:

(1) The carbon nanotube film structure 12 infiltrated by the liquid thermosetting polymer material 14 is gradually heated.

The valve 301 of the raw material input device 30 and the valve 501 of the raw material output device 50 are closed. The mold 40 is heated by a heating device to effect curing of the liquid thermosetting polymer material 14. The mold 40 is heated, and the thermosetting polymer material 14 is gradually heated and solidified. Since the temperature rise too fast during the solidification of the liquid thermosetting polymer material 14 causes the thermosetting polymer material 14 to swell and affect the material properties, the solidification of the liquid thermosetting polymer material 14 needs to be gradually increased. The curing temperature and curing time of the liquid thermosetting polymer material 14 are determined by the type and quality of the polymer material and the additive. The liquid thermosetting polymer material 14 has a curing temperature of less than 400 ° C and a curing time of less than 100 hours. The heating device may be one of a heating plate, a hot press, a flat vulcanizer, an autoclave or an oven.

(2) The carbon nanotube film structure 12 after gradually heating up is cooled to room temperature to obtain a carbon nanotube composite material 10.

After the thermosetting polymer material 14 is solidified and molded, the mold 40 is cooled to room temperature, and the carbon nanotube composite material 10 is obtained by demolding.

Embodiments of the present technical solution include an epoxy resin-containing thermosetting polymer material 14 The curing method specifically includes the following steps: First, a heating device is heated to 50 ° C to 70 ° C, at which temperature the thermosetting polymer material 14 containing epoxy resin is in a liquid state, and the temperature is maintained for 1 hour to 3 hours to make the thermosetting property. The polymer material 14 continues to absorb heat to increase its degree of solidification; secondly, the heating device is further heated to 80 ° C to 100 ° C, and maintained at this temperature for 1 hour to 3 hours, so that the thermosetting polymer material 14 continues to absorb heat to increase its Curing degree; again, further heating the heating device to 110 ° C ~ 150 ° C, maintaining at this temperature for 2 hours to 20 hours, so that the thermosetting polymer material 14 continues to absorb heat to increase its degree of solidification; finally, the heating device After cooling to room temperature, the mold 40 is taken out from the heating device, and a carbon nanotube composite material 10 is obtained by demolding.

Referring to FIG. 4 , the carbon nanotube composite material 10 provided by the embodiment of the present technical solution includes a thermosetting polymer material 14 and a carbon nanotube tube, and the carbon nanotube tube is uniformly distributed in the form of a carbon nanotube film structure 12 . In the thermosetting polymer material 14.

In summary, the present invention has indeed met the requirements of the invention patent, and has filed a patent application according to law. However, the above description is only a preferred embodiment of the present invention, and it is not possible to limit the scope of the patent application of the present invention. Equivalent modifications or variations made by persons skilled in the art in light of the spirit of the invention are intended to be included within the scope of the following claims.

10‧‧‧Nano Carbon Tube Composites

12‧‧‧Nano Carbon Tube Thin Film Structure

14‧‧‧Liquid thermosetting polymer materials

20‧‧‧Material supply device

30‧‧‧Material input device

40‧‧‧Mold

50‧‧‧Material output device

100‧‧‧Molding device

121‧‧‧First carbon nanotube layer

122‧‧‧Second carbon nanotube layer

123‧‧‧ third carbon nanotube layer

124‧‧‧ fourth carbon nanotube layer

201‧‧‧ container

202‧‧‧Import

203‧‧‧pressure port

301,501‧‧‧ valve

302‧‧‧ injection port

401‧‧‧Upper mold

402‧‧‧Mold

502‧‧‧Export

1 is a flow chart of a method for preparing a carbon nanotube composite material according to an embodiment of the present technical solution.

2 is a schematic structural view of a structure of a carbon nanotube film according to an embodiment of the present technical solution.

FIG. 3 is a schematic structural view of a carbon nanotube composite material forming apparatus according to an embodiment of the present technical solution.

4 is a schematic structural view of a carbon nanotube composite material according to an embodiment of the present technical solution.

12‧‧‧Nano Carbon Tube Thin Film Structure

121‧‧‧First carbon nanotube layer

122‧‧‧Second carbon nanotube layer

123‧‧‧ third carbon nanotube layer

124‧‧‧ fourth carbon nanotube layer

Claims (15)

A method for preparing a carbon nanotube composite material, comprising the steps of: preparing a self-supporting carbon nanotube film structure, the carbon nanotube film structure comprising a plurality of carbon nanotubes connected end to end, the plurality of nano tubes The carbon tube is oriented along a surface parallel to the surface of the carbon nanotube film structure; providing a liquid thermosetting polymer material; impregnating the carbon nanotube film structure with the liquid thermosetting polymer material; and curing the liquid thermosetting property The carbon nanotube film structure infiltrated by the polymer material obtains a carbon nanotube composite material, wherein the method for infiltrating the carbon nanotube film structure by the liquid thermosetting polymer material is injection infiltration, and specifically comprises the following steps : placing a carbon nanotube film structure in a mold; placing a liquid thermosetting polymer material in a container, and vacuuming the container until the vacuum degree of the container is lower than -0.09 MPa, The liquid thermosetting polymer material is applied with an injection pressure of 0.001 MPa to 10 MPa; and the liquid thermosetting polymer material is injected into the mold, and dipped The carbon nanotube film structure is moistened. The method for preparing a carbon nanotube composite material according to claim 1, wherein the method for preparing the carbon nanotube film structure comprises the steps of: providing a carbon nanotube array; and the nano carbon from the above Selecting a plurality of carbon nanotube segments of a certain width in the tube array; and Stretching the plurality of carbon nanotube segments perpendicular to the growth direction of the carbon nanotube array at a certain speed to obtain a continuous carbon nanotube film, wherein the arrangement of the carbon nanotubes in the carbon nanotube film is parallel to the above The direction of stretching. The method for preparing a carbon nanotube composite material according to the second aspect of the invention, wherein the method for preparing the carbon nanotube film structure further comprises the steps of: parallelizing at least two carbon nanotube films and not A carbon nanotube layer is obtained by gap laying; and at least two carbon nanotube layers are overlapped to form a carbon nanotube film structure. The method for preparing a carbon nanotube composite material according to claim 2, wherein the method for preparing the carbon nanotube film structure further comprises overlapping at least two carbon nanotube films to obtain one nanometer. The step of the carbon tube film structure. The method for preparing a carbon nanotube composite material according to claim 2, wherein the method for preparing the carbon nanotube film structure further comprises laying at least two carbon nanotube films in parallel and without gaps. A step of a carbon nanotube film structure. The method for preparing a carbon nanotube composite material according to claim 1, wherein the method further comprises the step of treating the carbon nanotube film structure with an organic solvent. The method for producing a carbon nanotube composite material according to claim 6, wherein the organic solvent is one or a mixture of ethanol, methanol, acetone, dichloroethane and chloroform. The method for preparing a carbon nanotube composite material according to claim 6, wherein the step of treating the carbon nanotube film structure by using the organic solvent The organic solvent is dropped on the surface of the carbon nanotube film structure through the test tube to infiltrate the entire carbon nanotube film structure. The method for preparing a carbon nanotube composite material according to claim 6, wherein the step of treating the carbon nanotube film structure by using the organic solvent comprises immersing the entire carbon nanotube film structure in an organic solvent. Infiltrated in the container. The method for preparing a carbon nanotube composite material according to claim 1, wherein the liquid thermosetting polymer material has a lower than 5 Pa at room temperature. The viscosity of seconds. The method for preparing a carbon nanotube composite material according to claim 1, wherein the thermosetting polymer material is a phenol resin, an epoxy resin, a bismaleimide resin, or a polybenzoxazine. A mixture of one or more of a resin, a cyanate resin, a polyimide resin, a polyurethane, a polymethyl methacrylate, and an unsaturated polyfluorene resin. The method for preparing a carbon nanotube composite material according to claim 1, wherein the liquid thermosetting polymer material infiltrates the carbon nanotube film structure for 10 minutes or longer. The method for preparing a carbon nanotube composite material according to claim 1, wherein the curing the carbon nanotube film structure infiltrated by the liquid thermosetting polymer material to obtain a carbon nanotube composite material The method specifically includes the steps of: gradually heating the carbon nanotube film structure impregnated with the liquid thermosetting polymer material to less than 400 ° C in less than 100 hours; and the carbon nanotube film structure after gradually heating up The temperature was cooled to room temperature to obtain a carbon nanotube composite material. Preparation method of the carbon nanotube composite material as described in claim 13 The method in which the structure of the carbon nanotube film infiltrated by the liquid thermosetting polymer material is gradually heated is realized by a heating device. The method for preparing a carbon nanotube composite material according to claim 14, wherein the heating device is a heating plate, a hot press, a flat vulcanizing machine, an autoclave or an oven.