CN111748177A - Preparation method of heat-resistant carbon nano paper/epoxy resin conductive composite material - Google Patents
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Abstract
A method for preparing a heat-resistant carbon nano paper/epoxy resin conductive composite material. The invention belongs to the field of heat-resistant composite materials. The invention aims to solve the technical problems of high brittleness and poor electric conductivity of the carbon nano paper prepared by the existing method. The method comprises the following steps: the invention takes multi-wall carbon nano-tubes as raw materials, triton as a dispersant and CMC as a binder to prepare carbon nano-paper, then takes the prepared carbon nano-paper as a reinforcement and epoxy resin as a matrix, and adopts a casting method to prepare the heat-resistant carbon nano-paper/epoxy resin conductive composite material. After the epoxy resin is added into the carbon nano paper prepared by the invention, the lowest resistivity of the composite material can reach 4.75 +/-0.15 omega-cm, the bending strength can reach 125.04 +/-5.62 MPa, the improvement is 71.23%, and the bending modulus can reach 5.83 +/-0.68 GPa, the improvement is 30.71%. The prepared carbon nano paper/epoxy resin conductive composite material can be applied to the fields of antistatic packaging materials, sensors, electrodes, capacitor materials and the like.
Description
Technical Field
The invention belongs to the field of heat-resistant composite materials; in particular to a preparation method of a heat-resistant carbon nano paper/epoxy resin conductive composite material.
Background
The conductive polymer composite material has attracted wide attention due to its excellent properties, and has wide applications in the fields of engineering and electronics, such as aerospace, electromagnetic shielding, electronic technology, and the like. Epoxy resin is the most widely used thermosetting polymer material, and is the most potential conductive polymer composite material matrix due to its excellent mechanical properties, good thermal stability, high chemical resistance, flame retardancy and other properties. The modification of the epoxy resin is an effective method for endowing the material with the conductivity, and can make up for the defects of high brittleness and poor crack propagation resistance of the epoxy resin.
Conventionally, metal powders of aluminum, gold, silver, copper, etc. have been widely used for the preparation of conductive polymer composites. However, such metal matrix composite materials have the disadvantages of easy oxidation, easy wave transmission of electromagnetic waves, high manufacturing cost and the like. Therefore, polymer composite materials containing carbonaceous fillers (carbon nanotubes, graphene, and carbon nanofibers) have received increasing attention for the preparation of conductive polymer materials due to their advantages of light weight, corrosion resistance, low cost, and easy processing. Among them, carbon nanotubes have a high specific surface area and excellent mechanical, electrical and optical properties, and are widely used in reinforcing materials for polymer composite materials. However, in the preparation process, it is very difficult to uniformly disperse the carbon nanotubes in the polymer matrix due to their strong agglomeration property, low solubility in the polymer matrix, and high viscosity of the resin. In recent years, carbon nanotubes are often assembled into micro or macro structures such as films, fibers and yarns to be applied, in order to solve the above problems. The carbon nano paper is also called as 'bucky paper', is a carbon nano tube macrostructure material with excellent multifunctional characteristics, and has good conductive performance, high specific modulus and specific strength. Compared with carbon nanotube powder, the carbon nanopaper is beneficial to avoiding the agglomeration of carbon nanotubes during the preparation of the composite material, thereby realizing better dispersion and higher concentration addition of the carbon nanotubes and further being beneficial to the formation of a high-conductivity network, and realizing the integration of the conductive/structural multifunctional composite material.
The vacuum filtration method is the most common method for preparing the carbon nano paper in laboratories and industries due to simple operation, sufficient raw materials and moderate cost. The method is that a suspension containing carbon nanotubes is first dispersed using a surfactant and then filtered using a vacuum filtration pump to induce the formation of carbon nanopaper. However, this method has a problem that the interconnection between the carbon nanotubes is weak due to the weak van der waals force between the carbon nanotubes, which affects the transfer of force and electrons in the carbon nanopaper, resulting in the carbon nanopaper having a large brittleness and a far different conductivity from the desired value. Therefore, the optimized preparation method of the carbon nano paper can not only improve the performance of the carbon nano paper, but also be beneficial to improving the overall performance of the carbon nano paper composite material.
Disclosure of Invention
The invention provides a preparation method of a heat-resistant carbon nano paper/epoxy resin conductive composite material, aiming at solving the technical problems of high brittleness and poor conductive capability of the carbon nano paper prepared by the existing method.
The preparation method of the heat-resistant carbon nano paper/epoxy resin conductive composite material is carried out according to the following steps:
dissolving CMC (sodium carboxymethylcellulose) in distilled water, and stirring at 70-90 ℃ for 50-70 min to obtain a CMC solution;
secondly, adding the multi-walled carbon nanotube and the triton X-100 into distilled water, and then carrying out ultrasonic dispersion treatment to obtain a uniformly dispersed multi-walled carbon nanotube suspension;
thirdly, transferring the multi-walled carbon nanotube suspension obtained in the second step onto a microporous filter membrane through vacuum filtration, and washing with deionized water to remove residual surfactant to obtain carbon nano paper;
transferring the CMC solution obtained in the first step onto the carbon nano paper obtained in the third step through vacuum filtration to obtain self-assembled CMC modified carbon nano paper, then placing the self-assembled CMC modified carbon nano paper at room temperature for vacuum drying, and separating the CMC modified carbon nano paper from a microporous filter membrane to obtain modified carbon nano paper;
fifthly, a casting molding process is adopted, 1-4 layers of modified carbon nano paper are placed at the bottom of a mold, then epoxy resin is added, the mold is closed after bubble removal treatment, pressurization is carried out, curing is carried out for 5-7 hours at the temperature of 100-140 ℃, and demolding is carried out after cooling to obtain the heat-resistant carbon nano paper/epoxy resin conductive composite material.
Further limiting, in the step one, the ratio of the mass of the CMC to the volume of the distilled water is (25-200) mg: 50 mL.
Further limiting, in step one, stirring is carried out at 80 ℃ for 60 min.
Further limiting, in the second step, the ratio of the mass of the multi-walled carbon nanotubes to the volume of the distilled water is (25-200) mg: 50 mL.
Further, in the second step, the mass ratio of the triton X-100 to the distilled water is (0.8-1.2): 100.
Further limiting, the parameters of the ultrasonic dispersion treatment in the second step are as follows: the ultrasonic power is 100W-300W, and the ultrasonic time is 20 min-40 min.
Further limiting, the parameters of the ultrasonic dispersion treatment in the second step are as follows: the ultrasonic power is 200W-250W, and the ultrasonic time is 30 min.
Further limiting, the aperture of the microporous filter membrane in the third step is 0.1-0.3 μm.
Further limiting, the pore diameter of the microporous filter membrane in the step three is 0.2 μm.
Further limiting, the mass ratio of the CMC to the multi-walled carbon nanotubes in the modified carbon nanopaper in the fourth step is 1: (0.8 to 1.2).
Further limiting, the mass ratio of the CMC to the multi-walled carbon nanotubes in the modified carbon nanopaper in the fourth step is 1: 1.
further limiting, the parameters of the bubble removing treatment in the fifth step are as follows: the temperature is 30-50 ℃, and the time is 20-40 min.
Further limiting, the parameters of the bubble removing treatment in the fifth step are as follows: the temperature is 40 deg.C, and the time is 30 min.
Further limiting, the mass ratio of the epoxy resin in the fifth step to the multi-walled carbon nanotubes in the second step is (1-30): 1.
further limiting, the mass ratio of the epoxy resin in the fifth step to the multi-walled carbon nanotubes in the second step is (5-20): 1.
compared with the prior art, the invention has the following remarkable effects:
the invention starts from the process of preparing carbon nano paper by a vacuum filtration method, and introduces carboxymethyl cellulose (CMC), which is a common adhesive in the papermaking technology, to help the carbon nano tube to form a film. Carboxymethyl cellulose is a typical cellulose derivative, has the characteristics of no smell, no toxicity, water solubility and the like, and is widely applied to the fields of flocculation, stability, petroleum drilling, food processing, drag reduction, detergents and the like. The carboxymethyl cellulose is particularly used in the field of papermaking, is used as a binder in textiles, is an ideal material for improving the performance of carbon nano paper and helping carbon nano tubes to form a film, is prepared into carbon nano paper, and is further used for preparing a conductive composite material by using carbon nano paper reinforced epoxy resin. The method has the following specific advantages:
1) the invention provides a method for modifying carbon nano paper, which combines paper making technology and material science technology to realize the improvement of the mechanical strength and the electrical conductivity of the carbon nano paper, and utilizes the carbon nano paper to prepare an epoxy conductive composite material, thereby endowing the epoxy composite material with the electrical conductivity and enhancing the heat resistance of the epoxy composite material, and the prepared carbon nano paper/epoxy composite material can be used as the conductive composite material to be applied to high-temperature environment.
2) The carbon nano-paper material with good mechanical property and high conductivity is formed by using the paper binder cellulose commonly used in the papermaking technology to assist the carbon nano-tube in film forming, and the method is also suitable for preparing film materials from other nano-materials such as graphene, carbon nano-fiber, MXenes and the like.
3) The invention provides a technology for preparing a conductive composite material by using carbon nano paper reinforced epoxy resin, the method can be popularized to other polymer composite materials, the method is simple to operate and low in cost, and the problem of easy agglomeration of carbon nano tubes in the polymer materials can be effectively solved.
4) After the epoxy resin is added into the carbon nano paper prepared by the invention, the lowest resistivity of the composite material can reach 4.75 +/-0.15 omega-cm, the bending strength can reach 125.04 +/-5.62 MPa, the improvement is 71.23%, and the bending modulus can reach 5.83 +/-0.68 GPa, the improvement is 30.71%. The prepared carbon nano paper/epoxy resin conductive composite material can be applied to the fields of antistatic packaging materials, sensors, electrodes, capacitor materials and the like. In addition, the carbon nanopaper/epoxy resin composite material can also be used in the field of high temperature resistant materials due to its good mechanical properties and excellent heat resistance.
Drawings
FIG. 1 is a surface topography of the carbon nanopaper after a third step of the embodiment;
FIG. 2 is a surface topography of the CMC modified carbon nanopaper after the fourth step in the first embodiment;
FIG. 3 is a bar graph showing the effect of CMC addition on the electrical properties of carbon nanopaper;
FIG. 4 is a graph of the effect of carbon nanotube content on electrical properties of carbon nanopaper;
FIG. 5 is a surface topography of a heat-resistant carbon nanopaper/epoxy conductive composite obtained in accordance with a first embodiment;
FIG. 6 is an enlarged view of FIG. 5 at area a;
fig. 7 is a graph showing the heat resistance of the heat-resistant carbon nanopaper/epoxy conductive composite obtained in the first embodiment and in the fourteenth to sixteenth embodiments;
fig. 8 is a graph illustrating the thermo-mechanical property test of the heat-resistant carbon nanopaper/epoxy conductive composite obtained in the first embodiment and in the fourteenth to sixteenth embodiments.
Detailed Description
The first embodiment is as follows: the preparation method of the heat-resistant carbon nanopaper/epoxy resin conductive composite material of the embodiment comprises the following steps:
firstly, dissolving 100mg of CMC (sodium carboxymethylcellulose) in 50mL of distilled water, and stirring for 60min at 80 ℃ to obtain a CMC solution;
secondly, adding 100mg of multi-walled carbon nanotubes and 0.2g of triton X-100 into 50mL of distilled water, and then performing ultrasonic dispersion treatment for 30min at 200W in an ultrasonic oscillator of a Palmer instrument (model: cp130pb) to obtain a uniformly dispersed multi-walled carbon nanotube suspension;
thirdly, transferring the multi-walled carbon nanotube suspension obtained in the second step to a microporous filter membrane with the pore diameter of 0.2 mu m through vacuum filtration, and washing with deionized water to remove residual surfactant to obtain carbon nano paper;
transferring the CMC solution obtained in the first step to the carbon nano paper obtained in the third step through vacuum filtration to obtain self-assembled CMC modified carbon nano paper, then placing the self-assembled CMC modified carbon nano paper at room temperature for vacuum drying for 24 hours, and then separating the CMC modified carbon nano paper from a microporous filter membrane to obtain modified carbon nano paper; the mass ratio of CMC to multi-walled carbon nanotubes in the modified carbon nanopaper is 1: 1;
fifthly, adopting a casting molding process, firstly placing 1 layer of modified carbon nano paper at the bottom of a mold, then adding 2g of epoxy resin, carrying out foam treatment for 30min at 40 ℃, closing the mold, pressurizing, curing for 6h at 120 ℃, cooling and demolding to obtain the heat-resistant carbon nano paper/epoxy resin conductive composite material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 10 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 50 mg. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 30 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 50 mg. Other steps and parameters are the same as those in the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 50 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 50 mg. Other steps and parameters are the same as those in the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 70 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 50 mg. Other steps and parameters are the same as those in the first embodiment.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 90 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 50 mg. Other steps and parameters are the same as those in the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 25 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 25 mg. Other steps and parameters are the same as those in the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 50 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 50 mg. Other steps and parameters are the same as those in the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 75 mg. And in the second step, the amount of the multi-wall carbon nano tubes is 75 mg. Other steps and parameters are the same as those in the first embodiment.
The detailed implementation mode is ten: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 125 mg. In the second step, the amount of the multi-wall carbon nano-tubes is 125 mg. Other steps and parameters are the same as those in the first embodiment.
The concrete implementation mode eleven: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 150 mg. In the second step, the amount of the multi-walled carbon nanotubes is 150 mg. Other steps and parameters are the same as those in the first embodiment.
The specific implementation mode twelve: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 175 mg. The amount of multi-walled carbon nanotubes in step two was 175 mg. Other steps and parameters are the same as those in the first embodiment.
The specific implementation mode is thirteen: the first difference between the present embodiment and the specific embodiment is: the amount of CMC in step one was 200 mg. In the second step, the amount of the multi-wall carbon nano-tubes is 200 mg. Other steps and parameters are the same as those in the first embodiment.
The specific implementation mode is fourteen: the first difference between the present embodiment and the specific embodiment is: and in the fifth step, the number of the modified carbon nano paper layers is 2. Other steps and parameters are the same as those in the first embodiment.
The concrete implementation mode is fifteen: the first difference between the present embodiment and the specific embodiment is: and in the fifth step, the number of the modified carbon nano paper layers is 3. Other steps and parameters are the same as those in the first embodiment.
The specific implementation mode is sixteen: the first difference between the present embodiment and the specific embodiment is: and in the fifth step, the number of the modified carbon nano paper layers is 4. Other steps and parameters are the same as those in the first embodiment.
Detection test
The surface topography of the carbon nanopaper after the third step of the first embodiment and the surface topography of the carbon nanopaper modified by the CMC after the fourth step are detected to obtain the surface topography of the carbon nanopaper after the third step of the first embodiment as shown in fig. 1, and obtain the surface topography of the carbon nanopaper modified by the CMC after the fourth step of the first embodiment as shown in fig. 2, as can be seen from fig. 1 and 2, the apparent topography of the carbon nanopaper is not affected by the addition of the CMC, but the carbon nanopaper is easily peeled from the microporous filter membrane, and the flexibility of the paper is enhanced.
(II) testing the conductivity of the CMC-modified carbon nano paper obtained in the second to the sixth steps to obtain a column diagram of the effect of the CMC addition amount on the electrical properties of the carbon nano paper as shown in FIG. 3. As seen from the diagram, the CMC content of the binder is increased, the carbon nano paper effectively helps the carbon nano tube network in the carbon nano paper to be lapped, so that the conductivity of the carbon nano paper is increased, and the resistivity is reduced. Therefore, the CMC added amount is about the same as the mass of the carbon nano-tube, and the obtained carbon nano-paper has the lowest resistivity.
And (iii) conducting performance of the CMC-modified carbon nanopaper obtained in the first embodiment and the seventh to thirteenth steps is tested, and a graph showing the influence of the amount of the carbon nanotubes on the electrical performance of the carbon nanopaper as shown in fig. 4 is obtained, and it can be seen from the graph that the carbon nanopaper prepared by using 100mg of the carbon nanotubes and adding the cellulose in the same proportion has the best conducting performance. At this time, the carbon nanotubes can just form complete carbon nanopaper, and under the action of cellulose, a complete and stable network structure is formed.
And (IV) detecting the surface topography of the heat-resistant carbon nanopaper/epoxy resin conductive composite material obtained in the first embodiment to obtain a surface topography map of the heat-resistant carbon nanopaper/epoxy resin conductive composite material obtained in the first embodiment as shown in fig. 5 and an enlarged view of an area a in fig. 5 as shown in fig. 6. As can be seen from fig. 5 and 6, the epoxy resin polymer is uniformly impregnated on the entire surface of the carbon nanopaper, indicating that the carbon nanopaper has good interaction and good compatibility with the epoxy resin.
Fifthly, the heat resistance of the heat-resistant carbon nanopaper/epoxy resin conductive composite material obtained in the first embodiment and the fourteenth to sixteenth embodiments is detected, and a heat resistance detection curve diagram of the heat-resistant carbon nanopaper/epoxy resin conductive composite material shown in fig. 7 is obtained, and it can be seen from the graph that the carbon nanopaper has good heat resistance, the temperature of the composite material with the fastest thermal decomposition rate gradually rises with the increase of the number of layers of the carbon nanopaper, and the mass residual rate also gradually rises when the temperature reaches 700 ℃. Therefore, the carbon nanopaper obviously enhances the heat resistance of the epoxy resin.
Sixthly, the thermomechanical properties of the heat-resistant carbon nanopaper/epoxy resin conductive composite material obtained in the first embodiment and the fourteenth to sixteenth embodiments are detected, and a thermomechanical property detection curve diagram of the heat-resistant carbon nanopaper/epoxy resin conductive composite material shown in fig. 8 is obtained, and it can be seen from the diagram that after the carbon nanopaper is added, the storage modulus of the epoxy resin composite material is obviously increased, and the glass transition temperature is also increased to a certain extent. The carbon nano paper endows the epoxy resin with the conductive functional characteristic, and obviously improves the mechanical property and the thermal mechanical property of the epoxy resin.
Claims (10)
1. A preparation method of a heat-resistant carbon nano paper/epoxy resin conductive composite material is characterized by comprising the following steps:
dissolving CMC in distilled water, and stirring at 70-90 ℃ for 50-70 min to obtain a CMC solution;
secondly, adding the multi-walled carbon nanotube and the triton X-100 into distilled water, and then carrying out ultrasonic dispersion treatment to obtain a uniformly dispersed multi-walled carbon nanotube suspension;
thirdly, transferring the multi-walled carbon nanotube suspension obtained in the second step onto a microporous filter membrane through vacuum filtration, and washing with deionized water to remove residual surfactant to obtain carbon nano paper;
transferring the CMC solution obtained in the first step onto the carbon nano paper obtained in the third step through vacuum filtration to obtain self-assembled CMC modified carbon nano paper, then placing the self-assembled CMC modified carbon nano paper at room temperature for vacuum drying, and separating the CMC modified carbon nano paper from a microporous filter membrane to obtain modified carbon nano paper;
fifthly, a casting molding process is adopted, 1-4 layers of modified carbon nano paper are placed at the bottom of a mold, then epoxy resin is added, the mold is closed after bubble removal treatment, pressurization is carried out, curing is carried out for 5-7 hours at the temperature of 100-140 ℃, and demolding is carried out after cooling to obtain the heat-resistant carbon nano paper/epoxy resin conductive composite material.
2. The method for preparing a heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the ratio of the mass of the CMC to the volume of the distilled water in the first step is (25-200) mg: 50 mL.
3. The method for preparing a heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein in the first step, the mixture is stirred at 80 ℃ for 60 min.
4. The method for preparing the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the ratio of the mass of the multi-walled carbon nanotubes to the volume of distilled water in the second step is (25-200) mg: 50 mL.
5. The method for preparing the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the mass ratio of the triton X-100 to the distilled water in the second step is (0.8-1.2): 100.
6. The method for preparing the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the parameters of the ultrasonic dispersion treatment in the second step are as follows: the ultrasonic power is 100W-300W, and the ultrasonic time is 20 min-40 min.
7. The method for preparing the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the pore size of the microporous filter membrane in the third step is 0.1 μm to 0.3 μm.
8. The method for preparing the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the mass ratio of the CMC in the modified carbon nanopaper to the multi-walled carbon nanotubes in the fourth step is 1: (0.8 to 1.2).
9. The method for preparing the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the parameters of the bubble removal treatment in the fifth step are as follows: the temperature is 30-50 ℃, and the time is 20-40 min.
10. The preparation method of the heat-resistant carbon nanopaper/epoxy resin conductive composite material as claimed in claim 1, wherein the mass ratio of the epoxy resin in the fifth step to the multi-walled carbon nanotubes in the second step is (1-30): 1.
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