CN111615318A - Preparation method and application of graphene/carbon nanotube composite porous membrane - Google Patents
Preparation method and application of graphene/carbon nanotube composite porous membrane Download PDFInfo
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- CN111615318A CN111615318A CN202010472601.8A CN202010472601A CN111615318A CN 111615318 A CN111615318 A CN 111615318A CN 202010472601 A CN202010472601 A CN 202010472601A CN 111615318 A CN111615318 A CN 111615318A
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- C01B32/15—Nano-sized carbon materials
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- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
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- C01B32/182—Graphene
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Abstract
The invention discloses a preparation method and application of a graphene/carbon nanotube composite porous membrane, and relates to the technical field of preparation of composite porous membranes, wherein the preparation method comprises the following steps: (1) dispersing crosslinked Polystyrene (PS) microspheres, graphene oxide and carboxylated carbon nanotubes in a solvent to obtain a suspension; (2) carrying out suction filtration on the suspension to obtain a filter membrane; (3) drying the filter membrane to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane; (4) and clamping the graphene oxide/carbon nano tube/PS microsphere composite membrane between graphite plates, and putting the graphite plates in an atmosphere furnace for carbonization to obtain the required graphene/carbon nano tube composite porous membrane. According to the invention, polystyrene microspheres are taken as a template, uniform and non-uniform dispersion of the polystyrene microspheres in the graphene/carbon nanotube composite membrane is realized through suction filtration, and the template is removed through low-temperature carbonization, so that low-temperature and simple preparation of the graphene/carbon nanotube composite porous membrane is realized.
Description
Technical Field
The invention relates to the technical field of preparation of composite porous membranes, and particularly relates to a preparation method and application of a graphene/carbon nanotube composite porous membrane.
Background
The rapid development of wireless communication technology has led to a rapid increase in the number of various highly integrated and high frequency electronic and electrical devices. The problems of electromagnetic pollution, electromagnetic interference, electromagnetic leakage and the like are increasingly prominent, and the health and the communication safety of a human body are seriously threatened. Electromagnetic shielding is an effective way to reduce electromagnetic radiation, improve electromagnetic compatibility, and prevent information leakage. The gigahertz (GHz) frequency band covers the important fields of military industry, mobile communication and the like, and the development and research of the electromagnetic shielding material aiming at the frequency band have extremely important application value in the military and civil fields.
Due to the high transverse-longitudinal ratio and excellent electric conduction and mechanical properties of graphene, graphene is often used as a basic unit to directly construct graphene-based macroscopic materials with continuous conductive framework structures, such as graphene paper, graphene foam, graphene aerogel and the like. A large number of results show that the electromagnetic shielding effectiveness of the graphene-based macroscopic material, especially the graphene-based carbon material, at 8.2-12.4GHz (X wave band) is as high as 30-50 decibels (dB) and far exceeds 20dB of the industrial standard. Nevertheless, such materials have the following two disadvantages: (1) the preparation process of the graphene-based carbon material usually involves high-temperature graphitization treatment at about 2000-3000 ℃ to endow the material with ultrahigh electric conduction and electromagnetic shielding performance, so that the preparation process has high requirements on equipment and high energy consumption; (2) the graphene-based carbon material with high conductivity has low dielectric loss, the shielding mechanism of electromagnetic waves mainly takes reflection as a main mechanism, and the reflected echoes can generate secondary pollution to the surrounding environment.
Disclosure of Invention
The invention provides a preparation method and application of a graphene/carbon nanotube composite porous membrane, and solves the problem of high requirements of the existing preparation process of graphene-based carbon materials.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of a graphene/carbon nanotube composite porous membrane comprises the following steps:
(1) dispersing crosslinked Polystyrene (PS) microspheres, graphene oxide and carboxylated carbon nanotubes in a solvent to obtain a suspension;
(2) carrying out suction filtration on the suspension to obtain a filter membrane;
(3) drying the filter membrane to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane;
(4) and clamping the graphene oxide/carbon nano tube/PS microsphere composite membrane between graphite plates, and putting the graphite plates in an atmosphere furnace for carbonization to obtain the required graphene/carbon nano tube composite porous membrane.
Preferably, the crosslinked Polystyrene (PS) microspheres account for 0-10 wt% of the total amount of the crosslinked Polystyrene (PS) microspheres, the graphene oxide and the carboxylated carbon nanotubes.
Preferably, the method comprises the following steps:
(1) dispersing the crosslinked Polystyrene (PS) microspheres with different concentrations, graphene oxide and carboxylated carbon nanotubes in a solvent to obtain suspensions containing the crosslinked Polystyrene (PS) microspheres with different concentrations;
(2) step-by-step suction filtration of the same amount of the suspension containing the crosslinked Polystyrene (PS) microspheres with different concentrations to obtain a filter membrane;
(3) drying the filter membrane to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane;
(4) and clamping the graphene oxide/carbon nano tube/PS microsphere composite membrane between graphite plates, and putting the graphite plates in an atmosphere furnace for carbonization to obtain the required graphene/carbon nano tube composite porous membrane.
Preferably, the drying conditions of the filter membrane in the step (3) are as follows: and (3) drying the filter membrane for 5-7 hours in an oven at the temperature of 85-95 ℃.
Preferably, the graphene oxide/carbon nanotube/PS microsphere composite membrane in step (4) is sandwiched between graphite plates, and is placed in an atmosphere furnace for carbonization treatment in an inert atmosphere.
Preferably, the graphene oxide is prepared by a Hummer method.
Preferably, the concentration of the graphene oxide and the carboxylated carbon nanotubes dispersed in the solvent in the step (1) is controlled to be 0.5-3 mg/mL.
Preferably, the carbonization treatment conditions in the step (4) are as follows: the temperature is 400-.
Preferably, the prepared graphene/carbon nanotube composite porous film has the thickness of 50-110 mu m and the density of 0.05-0.16g/cm3。
The graphene/carbon nanotube composite porous membrane prepared by the preparation method is applied to electronic and electrical equipment as a patch for shielding electromagnetic waves.
By adopting the technical scheme, the polystyrene microspheres are taken as the template, the uniform/non-uniform dispersion of the polystyrene microspheres in the graphene/carbon nanotube composite membrane is realized by suction filtration, and the template is removed by low-temperature carbonization, so that the low-temperature and simple preparation of the graphene/carbon nanotube composite porous membrane is realized. On one hand, the pi-pi interaction between the one-dimensional carbon nanotube and the two-dimensional graphene nanosheet is beneficial to the rapid construction of a conductive network in the material, and the temperature of the carbonization process is reduced. On the other hand, various cell structures in the composite film are beneficial to reducing the reflection loss of electromagnetic waves on the surface of the material and enhancing the absorption loss of the electromagnetic waves in the material. Therefore, on the premise of ensuring excellent electromagnetic shielding performance of the material, the wave absorbing performance of the graphene-based carbon material is improved, and the application of the graphene-based carbon material in microelectronic devices is promoted.
Drawings
FIG. 1 is a scanning electron microscope image of a cross section of a graphene/carbon nanotube composite porous membrane prepared by the method of the present invention;
fig. 2 is a scanning electron microscope image of the surface of the graphene/carbon nanotube composite porous membrane prepared by the method of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
Dispersing 15mg of crosslinked Polystyrene (PS) microspheres (with the particle size of 1-10 microns), 0.15g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring to obtain a suspension; carrying out suction filtration on 50mL of suspension to obtain a filter membrane; drying the filter membrane in an oven at 90 ℃ for 6 hours to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane; and clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphite plates in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 700 ℃, the heating rate is 3 ℃/min, and the treatment time is 1h, so that the required graphene/carbon nanotube composite porous membrane is obtained.
The raw materials used in the present invention are all commercially available products.
As shown in FIGS. 1 and 2, the prepared graphene/carbon nanotube composite porous membrane has a thickness of about 60 μm and a density of 0.09g/cm3And the electromagnetic shielding performance of the vector network analyzer in the X wave band is tested by a waveguide method, and the obtained electromagnetic shielding efficiency is 36 dB.
Example 2
Dispersing 0.3g of graphene oxide and 0.05g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring to obtain a suspension; carrying out suction filtration on 50mL of suspension to obtain a filter membrane; drying the filter membrane in an oven at 85 ℃ for 5 hours to obtain a graphene oxide/carbon nanotube composite membrane; and clamping the graphene oxide/carbon nanotube-composite membrane between graphite plates, and putting the graphite plates in an atmosphere furnace for carbonization in an inert atmosphere at the temperature of 400 ℃, the heating rate of 2 ℃/min and the treatment time of 0.5h to obtain the required graphene/carbon nanotube composite porous membrane.
The prepared graphene/carbon nano tube composite porous film has the thickness of about 50 mu m and the density of 0.16g/cm3. The electromagnetic shielding performance of the vector network analyzer in the X wave band is tested by a waveguide method, and the obtained electromagnetic shielding effectiveness is 30 dB.
Example 3
Dispersing 50mg of crosslinked Polystyrene (PS) microspheres (with the particle size of 1-10 mu m), 0.3g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring to obtain a suspension; carrying out suction filtration on 50mL of suspension to obtain a filter membrane; drying the filter membrane in an oven at 95 ℃ for 7 hours to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane; and clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphite plates in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 1000 ℃, the heating rate is 4 ℃/min, and the treatment time is 1.5h, so that the required graphene/carbon nanotube composite porous membrane is obtained.
The prepared graphene/carbon nano tube composite porous membrane has the thickness of about 70 mu m and the density of 0.07g/cm3. The electromagnetic shielding performance of the vector network analyzer in the X wave band is tested by a waveguide method, and the obtained electromagnetic shielding efficiency is 42 dB.
Example 4
The foaming rate of the graphene/carbon nanotube composite porous membrane can be realized by regulating the content of the PS microspheres, so that the density of the graphene/carbon nanotube composite porous membrane is reduced along with the increase of the content of the PS microspheres. In order to research the influence of the gradient cell structure on the shielding performance of the material, suspensions of crosslinked Polystyrene (PS) microspheres, graphene oxide and carboxylated carbon nanotubes with different PS microsphere contents (0, 2, 4.5, 6 and 10 wt%) are prepared, and are subjected to step-by-step suction filtration, drying and carbonization to obtain the graphene/carbon nanotube composite porous membrane with different hierarchical structures.
Preparing a suspension with the PS microsphere content of 0 wt% for standby: dispersing 0.15g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring;
preparing a suspension with PS microsphere content of 2 wt% for standby: dispersing 6.1mg of crosslinked Polystyrene (PS) microspheres (with the particle size of 1-10 microns), 0.15g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring;
preparing a suspension with the PS microsphere content of 4.5 wt% for standby: dispersing 14.1mg of crosslinked Polystyrene (PS) microspheres (with the particle size of 1-10 microns), 0.15g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring;
preparing a suspension with 6 wt% of PS microspheres for later use: dispersing 19.5mg of crosslinked Polystyrene (PS) microspheres (with the particle size of 1-10 microns), 0.15g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring;
preparing a suspension with a PS microsphere content of 10 wt% for use: dispersing 33.3mg of crosslinked Polystyrene (PS) microspheres (with the particle size of 1-10 microns), 0.15g of graphene oxide and 0.15g of carboxylated carbon nanotubes in 100mL of deionized water by ultrasonic and magnetic stirring;
preparing the following graphene/carbon nanotube composite porous membrane with a multilayer structure:
a first group: positive gradient: the content of PS microspheres is 0-0-2-2-6-6-10-10: respectively taking 10mL of the prepared suspension with the PS microsphere content of 0 wt%, the suspension with the PS microsphere content of 2 wt% and the suspension with the PS microsphere content of 6 wt% and the suspension with the PS microsphere content of 10 wt%, sequentially performing suction filtration, wherein the subsequent suction filtration is to superpose the previous suction filtration to obtain a multi-layer filter membrane, and placing the multi-layer filter membrane in an oven to dry for 6 hours at 90 ℃ to obtain the graphene oxide/carbon nanotube/PS microsphere composite membrane; clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphene oxide/carbon nanotube/PS microsphere composite membrane in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 700 ℃, the heating rate is 3 ℃/min, and the treatment time is 1h, so that the required graphene/carbon nanotube composite porous membrane with a multilayer structure is obtained;
second group: negative gradient: the content of PS microspheres is 10-10-6-6-2-2-0-0: respectively taking 10mL of the prepared suspension with the PS microsphere content of 10 wt%, the suspension with the PS microsphere content of 6 wt% and the suspension with the PS microsphere content of 2 wt% and the suspension with the PS microsphere content of 0 wt%, sequentially performing suction filtration, wherein the subsequent suction filtration is to superpose the previous suction filtration to obtain a multi-layer filter membrane, and placing the multi-layer filter membrane in an oven to dry for 6 hours at 90 ℃ to obtain the graphene oxide/carbon nanotube/PS microsphere composite membrane; clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphene oxide/carbon nanotube/PS microsphere composite membrane in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 700 ℃, the heating rate is 3 ℃/min, and the treatment time is 1h, so that the required graphene/carbon nanotube composite porous membrane with a multilayer structure is obtained;
third group: positive-double gradient: the content of PS microspheres is 0-2-6-10-10-6-2-0: respectively taking 10mL of the prepared suspension with the PS microsphere content of 0 wt%, the suspension with the PS microsphere content of 2 wt%, the suspension with the PS microsphere content of 6 wt%, the suspension with the PS microsphere content of 10 wt%, the suspension with the PS microsphere content of 6 wt% and the suspension with the PS microsphere content of 2 wt% and the suspension with the PS microsphere content of 0 wt%, sequentially carrying out suction filtration, wherein the subsequent suction filtration is carried out on the basis of the previous suction filtration to obtain a multi-layer filter membrane, and drying the multi-layer filter membrane in an oven at 90 ℃ for 6 hours to obtain the graphene oxide/carbon nanotube/PS microsphere composite membrane; clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphene oxide/carbon nanotube/PS microsphere composite membrane in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 700 ℃, the heating rate is 3 ℃/min, and the treatment time is 1h, so that the required graphene/carbon nanotube composite porous membrane with a multilayer structure is obtained;
and a fourth group: negative-double gradient: the content of PS microspheres is 10-6-2-0-0-2-6-10: respectively taking 10mL of the prepared suspension with the PS microsphere content of 10 wt%, the suspension with the PS microsphere content of 6 wt%, the suspension with the PS microsphere content of 2 wt%, the suspension with the PS microsphere content of 0 wt%, the suspension with the PS microsphere content of 2 wt% and the suspension with the PS microsphere content of 6 wt% and the suspension with the PS microsphere content of 10 wt%, sequentially carrying out suction filtration, wherein the subsequent suction filtration is carried out on the basis of the previous suction filtration to obtain a multi-layer filter membrane, and drying the multi-layer filter membrane in an oven at 90 ℃ for 6 hours to obtain the graphene oxide/carbon nanotube/PS microsphere composite membrane; clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphene oxide/carbon nanotube/PS microsphere composite membrane in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 700 ℃, the heating rate is 3 ℃/min, and the treatment time is 1h, so that the required graphene/carbon nanotube composite porous membrane with a multilayer structure is obtained;
control group: the content of PS microspheres is 4.5 wt%: taking 80mL of the prepared suspension with the PS microsphere content of 4.5 wt% for suction filtration to obtain a filter membrane, and drying the filter membrane in a drying oven at 90 ℃ for 6 hours to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane; and clamping the graphene oxide/carbon nanotube/PS microsphere composite membrane between graphite plates, and placing the graphite plates in an atmosphere furnace for carbonization treatment in an inert atmosphere, wherein the temperature is 700 ℃, the heating rate is 3 ℃/min, and the treatment time is 1h, so that the required graphene/carbon nanotube composite porous membrane is obtained.
The electromagnetic shielding performance of the prepared graphene/carbon nanotube composite porous membrane with the multilayer structure (the thickness is about 110 μm) in the X wave band is tested on a vector network analyzer by a waveguide method, three samples are tested for each structure, and an average value is taken. As a result, it was found that the electromagnetic shielding effectiveness of the first group to the fourth group was not greatly different, about 80 dB. Therefore, different gradient structure designs have little influence on the density and the electromagnetic shielding performance of the graphene/carbon nanotube composite film, but have great influence on the electromagnetic shielding mechanism. The third group of materials with positive-double gradient structures has the strongest wave-absorbing performance, more than 60% of electromagnetic wave energy is absorbed, and less than 40% of electromagnetic wave energy is reflected; the wave-absorbing performance of the first group of materials with the positive gradient structure is inferior, and then the uniform structure of the negative gradient of the second group and the contrast group is adopted, and the structure with the worst wave-absorbing performance is designed into a negative-double gradient structure of the fourth group.
By the method, the heat treatment temperature of the graphene-based carbon material can be effectively reduced on the premise of ensuring the electromagnetic shielding performance of the material, and the low-cost preparation of the material is realized; meanwhile, the dielectric property of the graphene/carbon nanotube composite film can be continuously changed through the gradient cell structure, the wave absorbing property of the graphene-based carbon material is improved, the impedance matching of electromagnetic waves on the surface of the material and the air is improved, the reflection loss of the electromagnetic waves on the surface of the material is reduced, the absorption loss of the electromagnetic waves in the material is enhanced, and the secondary pollution of the electromagnetic waves is effectively inhibited.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. A preparation method of a graphene/carbon nanotube composite porous membrane is characterized by comprising the following steps: the method comprises the following steps:
(1) dispersing crosslinked Polystyrene (PS) microspheres, graphene oxide and carboxylated carbon nanotubes in a solvent to obtain a suspension;
(2) carrying out suction filtration on the suspension to obtain a filter membrane;
(3) drying the filter membrane to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane;
(4) and clamping the graphene oxide/carbon nano tube/PS microsphere composite membrane between graphite plates, and putting the graphite plates in an atmosphere furnace for carbonization to obtain the required graphene/carbon nano tube composite porous membrane.
2. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: the crosslinked Polystyrene (PS) microspheres account for 0-10 wt% of the total amount of the crosslinked Polystyrene (PS) microspheres, the graphene oxide and the carboxylated carbon nanotubes.
3. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: the method comprises the following steps:
(1) dispersing the crosslinked Polystyrene (PS) microspheres with different concentrations, graphene oxide and carboxylated carbon nanotubes in a solvent to obtain suspensions containing the crosslinked Polystyrene (PS) microspheres with different concentrations;
(2) step-by-step suction filtration of the same amount of the suspension containing the crosslinked Polystyrene (PS) microspheres with different concentrations to obtain a filter membrane;
(3) drying the filter membrane to obtain a graphene oxide/carbon nanotube/PS microsphere composite membrane;
(4) and clamping the graphene oxide/carbon nano tube/PS microsphere composite membrane between graphite plates, and putting the graphite plates in an atmosphere furnace for carbonization to obtain the required graphene/carbon nano tube composite porous membrane.
4. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: the drying conditions of the filter membrane in the step (3) are as follows: and (3) drying the filter membrane for 5-7 hours in an oven at the temperature of 85-95 ℃.
5. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: and (4) clamping the graphene oxide/carbon nano tube/PS microsphere composite membrane between graphite plates, and placing the graphene oxide/carbon nano tube/PS microsphere composite membrane in an atmosphere furnace for carbonization treatment in inert atmosphere.
6. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: the graphene oxide is prepared by a Hummer method.
7. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: and (2) controlling the concentration of the graphene oxide and the carboxylated carbon nano tube after being dispersed in the solvent in the step (1) to be 0.5-3 mg/mL.
8. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: the carbonization treatment conditions in the step (4) are as follows: the temperature is 400-.
9. The method for preparing a graphene/carbon nanotube composite porous membrane according to claim 1, wherein: the prepared graphene/carbon nano tube composite porous film has the thickness of 50-110 mu m and the density of 0.05-0.16g/cm3。
10. A graphene/carbon nanotube composite porous film prepared by the method for preparing a graphene/carbon nanotube composite porous film according to any one of claims 1 to 9, wherein: the graphene/carbon nanotube composite porous membrane is used as a patch for shielding electromagnetic waves and applied to electronic and electrical equipment.
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