CN112210766A - Carbon nanotube foam material with electromagnetic shielding performance and preparation method and application thereof - Google Patents
Carbon nanotube foam material with electromagnetic shielding performance and preparation method and application thereof Download PDFInfo
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- CN112210766A CN112210766A CN201910629222.2A CN201910629222A CN112210766A CN 112210766 A CN112210766 A CN 112210766A CN 201910629222 A CN201910629222 A CN 201910629222A CN 112210766 A CN112210766 A CN 112210766A
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Abstract
The invention discloses a carbon nano tube foam material with electromagnetic shielding performance and a preparation method and application thereof. The preparation method of the carbon nano tube foam material with the electromagnetic shielding performance comprises the following steps: placing carbon nanotube foam in a reaction chamber of a chemical vapor deposition apparatus; and heating the reaction chamber to 1000-1100 ℃, and then at least introducing a carbon source and a reducing gas into the reaction chamber, so as to perform secondary deposition of amorphous carbon on the carbon nanotube foam, thereby obtaining the carbon nanotube foam material with the electromagnetic shielding performance, wherein the carbon nanotube foam material comprises a porous structure consisting of a 3D network structure with self-supporting capability. The carbon nanotube foam material with the electromagnetic shielding performance has excellent shielding efficiency, controllable density and thickness, small mass, good flexibility and excellent stability of the shielding efficiency; and the preparation process is simple, and the batch production can be expanded.
Description
Technical Field
The invention relates to a preparation method of an electromagnetic shielding material, in particular to a carbon nano tube foam material with electromagnetic shielding performance, a preparation method and application thereof, and belongs to the technical field of composite materials.
Background
With the proliferation of electronic systems and electronic devices, such as wireless networks and personal electronic devices, electromagnetic interference (EMI) has also increased exponentially. Electronic devices are now used which are characterized by high power, small size and fast operation speed, but this also means that more electromagnetic waves are emitted which not only interfere with the operation of adjacent devices or systems (e.g. aircraft), but also pose a potential health risk to humans. In addition, data theft and hardware security breaches are common, and therefore better and more secure electromagnetic shielding is needed to enhance digital privacy. Finally, with the advent of flexible electronic devices, wearable devices, and implantable biomedical systems, EMI shielding materials must be ultra-thin, ultra-light, and flexible to meet current needs.
The electromagnetic shielding materials reported at present have certain limitations. Conventional metal materials such as metals and metal alloys are common EMI shielding materials due to their excellent electrical conductivity. However, metals are poor in ductility and flexibility, and are dense, heavy, susceptible to corrosion, and difficult to process, which further limits their further use in modern EMI shielding materials. In addition, due to the characteristics of low cost, small density, easy molding and the like of the conductive high-molecular electromagnetic shielding material such as a polymer material, the conductive nano particles are dispersed in the insulating polymer matrix in proper concentration, and a conductive network is formed in the polymer through the conductive nano particles, so that the radiated electromagnetic waves can be reflected and absorbed, and the composite electromagnetic shielding material is obtained. However, in order to obtain high electromagnetic shielding effectiveness, the conductive nanoparticles are loaded in a large amount, but the high loading causes agglomeration of the conductive particles, which degrades the mechanical properties of the shielding material. In summary, the conventional metallic shielding material cannot satisfy the requirement of light weight. Although the conductive polymer shielding material has a certain shielding effectiveness, high shielding effectiveness and good mechanical properties cannot be obtained at the same time, and the dispersibility of the conductive filler in the polymer material is poor.
Disclosure of Invention
The invention mainly aims to provide a carbon nano tube foam material with electromagnetic shielding performance and a preparation method thereof, so as to overcome the defects in the prior art.
The invention also aims to provide application of the carbon nano tube foam material with the electromagnetic shielding property.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a carbon nano tube foam material with electromagnetic shielding performance, which comprises the following steps:
providing a carbon nanotube foam;
providing a carbon nanotube foam;
placing the carbon nanotube foam in a reaction chamber of a chemical vapor deposition apparatus;
and heating the reaction chamber to 1000-1100 ℃, and then at least introducing a carbon source and a reducing gas into the reaction chamber, so as to perform secondary deposition of amorphous carbon on the carbon nanotube foam, thereby obtaining the carbon nanotube foam material with the electromagnetic shielding performance, wherein the carbon nanotube foam material comprises a porous structure consisting of a 3D network structure with self-supporting capability.
In some embodiments, the method of making comprises:
placing carbon nanotube foam into the reaction chamber;
introducing inert gas serving as carrier gas into the reaction chamber to discharge air in the reaction chamber;
and when the temperature in the reaction chamber is raised to 1000-1100 ℃, introducing carrier gas, a carbon source and reducing gas into the reaction chamber, preserving the heat for 10-60 min, and then cooling to obtain the carbon nano tube foam material with the electromagnetic shielding performance.
The embodiment of the invention also providesThe carbon nano tube foam material with the electromagnetic shielding performance prepared by the method comprises a porous structure consisting of a 3D network structure with self-supporting capacity, wherein the porosity of the porous structure is 92-96%, the pore diameter of pores contained in the porous structure is 10 nm-300 mu m, and the density is 0.017-0.077 g/cm3The thickness of the carbon nanotube foam material is 0.5-5 mm, and the shielding effectiveness of the X wave band is 50-102 dB.
The embodiment of the invention also provides application of the carbon nano tube foam material with the electromagnetic shielding performance in preparing the electromagnetic shielding material.
Compared with the prior art, the invention has the beneficial effects that:
1) the carbon nanotube foam material with the electromagnetic shielding performance has excellent shielding efficiency, controllable density and thickness, small mass, good flexibility and excellent stability of the shielding efficiency;
2) the thickness of the carbon nano tube foam material with the electromagnetic shielding performance can be regulated and controlled by a simple method, and the density can be regulated and controlled by deposition time;
3) the materials used in the invention are carbon nanotube foam, carbon sources such as ethylene and the like, reducing gases such as hydrogen and the like, inert gases such as argon and the like, toxic and dangerous articles are not used, and the concept of environmental protection is met;
4) the preparation method has the advantages of simple preparation process and low cost, and can enlarge batch production and realize productization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart illustrating a process for preparing a carbon nanotube foam with electromagnetic shielding properties according to an exemplary embodiment of the present invention.
Fig. 2 is an SEM image of a carbon nanotube foam with electromagnetic shielding properties in an exemplary embodiment of the invention.
Fig. 3 is a schematic diagram illustrating bending of a carbon nanotube foam material with electromagnetic shielding performance according to an exemplary embodiment of the present invention.
Fig. 4 a-4 f are micro-topography images of the original carbon nanotube foam, obtained with different deposition times, respectively, of the carbon nanotube foam material with electromagnetic shielding performance in an exemplary embodiment of the invention.
FIG. 5a is a graph of the shielding effectiveness of carbon nanotube foam in X-band with different thickness and the same deposition time (20min) in an exemplary embodiment of the invention.
FIG. 5b is a graph of the shielding effectiveness of carbon nanotube foam of the same thickness (1mm) at different deposition times in the X-band according to an exemplary embodiment of the present invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide a solution for preparing a carbon nanotube foam having electromagnetic shielding properties by a CVD (i.e., chemical vapor deposition) method. The technical solution, its implementation and principles, etc. will be further explained as follows.
The carbon nanotube is a one-dimensional nanomaterial formed by curling a single-layer or multi-layer graphite sheet layer, has a unique structure and a plurality of excellent physical properties such as light weight, excellent mechanical properties, good structural flexibility, chemical stability and high temperature resistance, and particularly has the important point that the carbon nanotube is the best shielding material compared with an electromagnetic shielding material thereof. Therefore, the light weight, flexibility and high conductivity of the carbon nanotube determine that the carbon nanotube is expected to be an ideal material for novel electromagnetic shielding.
The preparation principle of the invention is as follows: the invention utilizes carbon nanotube foam grown by a floating CVD method, takes ethylene and the like as carbon sources, and introduces carriers and carbon sources to carry out secondary deposition of amorphous carbon on the original carbon nanotube foam. After the secondary deposition, the carbon nanotube foam is changed into a 3D network structure with self-supporting capability from an original network structure which is easy to collapse. Due to the excellent conductivity of the carbon nano tube, the foam has high reflection to electromagnetic waves, the rest electromagnetic waves enter the foam, and the porous structure of the foam can enable the electromagnetic waves to be reflected for multiple times inside and dissipated inside, so that the high absorption efficiency is achieved.
One aspect of the embodiments of the present invention provides a method for preparing a carbon nanotube foam material with electromagnetic shielding performance, which includes:
providing a carbon nanotube foam;
placing the carbon nanotube foam in a reaction chamber of a chemical vapor deposition apparatus;
and heating the reaction chamber to 1000-1100 ℃, and then at least introducing a carbon source and a reducing gas into the reaction chamber, so as to perform secondary deposition of amorphous carbon on the carbon nanotube foam, thereby obtaining the carbon nanotube foam material with the electromagnetic shielding performance, wherein the carbon nanotube foam material comprises a porous structure consisting of a 3D network structure with self-supporting capability.
In some embodiments, the method of making specifically comprises:
placing carbon nanotube foam into the reaction chamber;
introducing inert gas serving as carrier gas into the reaction chamber to discharge air in the reaction chamber;
and when the temperature in the reaction chamber is raised to 1000-1100 ℃, introducing carrier gas, a carbon source and reducing gas into the reaction chamber, preserving the heat for 10-60 min, and then cooling to obtain the carbon nano tube foam material with the electromagnetic shielding performance.
In the invention, the reaction time of deposition can regulate and control the density of the finally obtained carbon nanotube foam material, and the longer the deposition time is, the higher the density of the carbon nanotube foam material is.
Furthermore, the porosity of the porous structure is 92-96%, the aperture of the pores is 10 nm-300 μm, and the density is 0.017-0.077 g/cm3。
In some embodiments, the method of making comprises: and preparing the carbon nano tube foam at least by adopting a floating catalytic chemical vapor deposition method.
Further, the density of the carbon nano tube foam is 0.007-0.009 g/cm3The thickness is 2-2.5 cm.
In some embodiments, the method of making comprises: and heating the temperature in the reaction chamber to 1000-1100 ℃ at a heating rate of 5-15 ℃/min.
In some embodiments, the mass ratio of secondarily deposited amorphous carbon to carbon nanotube foam is 108: 89-768: 89.
further, the carbon source for the second deposition may be a gas phase carbon source such as ethylene, etc., or a liquid phase carbon source such as ethanol, toluene, etc., but is not limited thereto.
Further, the reducing gas may be hydrogen, but is not limited thereto,
further, the inert gas may be Ar, but is not limited thereto,
in some embodiments, the method of making comprises: and introducing the carrier gas into the reaction chamber at a rate of 200-250 sccm.
Further, the preparation method comprises the following steps: and introducing the reducing gas into the reaction chamber at a rate of 200-250 sccm.
Further, the preparation method comprises the following steps: and introducing the reducing gas and the carbon source into the reaction chamber at the rates of 120-160 sccm and 60-80 sccm respectively.
The embodiment of the invention also provides the carbon nanotube foam material with the electromagnetic shielding property prepared by the method, which comprises a porous structure consisting of a 3D network structure with self-supporting capacity, wherein the porosity of the porous structure is 92-96%, the pore diameter of pores contained in the porous structure is 10 nm-300 mu m, and the density is 0.017-0.077 g/cm3The thickness of the carbon nanotube foam material is 0.5-5 mm, and the shielding effectiveness of the X wave band is 50-102 dB.
In another aspect of the embodiments of the present invention, an application of the carbon nanotube foam material with electromagnetic shielding performance in preparing an electromagnetic shielding material is also provided.
In conclusion, the carbon nanotube foam material with the electromagnetic shielding performance has excellent shielding efficiency, controllable density and thickness, small mass, good flexibility and excellent stability of the shielding efficiency; moreover, the preparation process is simple, the cost is low, the batch production can be expanded, and the commercialization is realized.
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
1) original carbon nanotube foam: the carbon nanotube fibers produced by floating CVD were collected and wound on a collection shaft.
2) Sample preparation: the original carbon nanotube foam was cut into regular rectangles with a laser.
3) Preparing original carbon nanotube foams with different thicknesses: shims (1mm, 2mm, 3mm, 5mm, 10mm) with standard dimensions were prepared and the original carbon nanotube foam was pressed to different thicknesses, respectively.
4) Secondary deposition: putting the foam in the step 3) into a quartz boat, pushing the quartz boat into the middle of the quartz tube, mounting flanges at two ends of the quartz tube, and introducing argon to remove air in the quartz tube. The argon flow is 200-250 sccm, the temperature is raised to 1000-1100 ℃ at the speed of 10 ℃/min, and the hydrogen and ethylene valves are opened, wherein the flow is 120-160 sccm and 60-80 sccm respectively. The reaction time is 10min, 20min, 30min, 40min and 60min respectively. And (3) closing the hydrogen and ethylene valves after the reaction time is over, naturally cooling the tube furnace to room temperature, taking out the quartz boat, and obtaining the final carbon nanotube foam material with the electromagnetic shielding performance, wherein the test data of the thickness, the density and the like are shown in the table 1 and the table 2.
TABLE 11 Shielding effectiveness and Density of carbon nanotube foams of different deposition times in mm thickness
TABLE 2 Shielding effectiveness and Density of carbon nanotube foams of different thicknesses deposited for 20min
| t(cm) | ρ(g/cm3) | SE(dB) |
| 0.05 | 0.035 | 63.83305 |
| 0.08 | 0.018 | 79.41215 |
| 0.1 | 0.015 | 84.15 |
| 0.2 | 0.02 | 92.69666 |
| 0.3 | 0.02 | 102.7261 |
| 0.5 | 0.066 | 102.7483 |
Through testing, the SEM images of the carbon nanotube foam material with electromagnetic shielding performance obtained in this example can be seen in fig. 2, and the microscopic morphology images of the original carbon nanotube foam material and the carbon nanotube foam material with electromagnetic shielding performance obtained at different deposition times can be seen in fig. 4 a-4 f, which have excellent shielding performance (for example, see fig. 5a, which shows the shielding performance of the carbon nanotube foam with different thicknesses and the same deposition time (20min) in the X-band, and see fig. 5b, which shows the shielding performance of the carbon nanotube foam with the same thickness (1mm) and the different deposition times in the X-band), small mass, good flexibility (see fig. 3), and excellent stability of the shielding performance.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
Unless specifically stated otherwise, use of the terms "comprising", "including", "having" or "having" is generally to be understood as open-ended and not limiting.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (11)
1. A preparation method of a carbon nano tube foam material with electromagnetic shielding performance is characterized by comprising the following steps:
providing a carbon nanotube foam;
placing the carbon nanotube foam in a reaction chamber of a chemical vapor deposition apparatus;
and heating the reaction chamber to 1000-1100 ℃, and then at least introducing a carbon source and a reducing gas into the reaction chamber, so as to perform secondary deposition of amorphous carbon on the carbon nanotube foam, thereby obtaining the carbon nanotube foam material with the electromagnetic shielding performance, wherein the carbon nanotube foam material comprises a porous structure consisting of a 3D network structure with self-supporting capability.
2. The production method according to claim 1, characterized by comprising:
placing carbon nanotube foam into the reaction chamber;
introducing inert gas serving as carrier gas into the reaction chamber to discharge air in the reaction chamber;
when the temperature in the reaction chamber is raised to 1000-1100 ℃, introducing carrier gas, a carbon source and reducing gas into the reaction chamber, preserving the heat for 10-60 min, and then cooling to obtain the carbon nanotube foam material with the electromagnetic shielding performance;
and/or the porosity of the porous structure is 92-96%, the aperture of the contained holes is 10 nm-300 mu m, and the density is 0.017-0.077 g/cm3。
3. The production method according to claim 1, characterized by comprising: and preparing the carbon nano tube foam at least by adopting a floating catalytic chemical vapor deposition method.
4. The method according to claim 1 or 2, characterized by comprising: heating the temperature in the reaction chamber to 1000-1100 ℃ at a heating rate of 5-15 ℃/min; and/or the mass ratio of the amorphous carbon deposited twice to the carbon nanotube foam is 108: 89-768: 89.
5. the method according to claim 1 or 2, characterized in that: the carbon source comprises a gas phase carbon source and/or a liquid phase carbon source; preferably, the source of the gas phase carbon source comprises ethylene; preferably, the source of the liquid-phase carbon source comprises ethanol and/or toluene.
6. The method according to claim 1 or 2, characterized in that: the reducing gas comprises hydrogen.
7. The method according to claim 1 or 2, characterized in that: the inert gas comprises Ar.
8. The method of claim 2, comprising: introducing the carrier gas into the reaction chamber at a rate of 200-250 sccm; and/or the reducing gas is introduced into the reaction chamber at a rate of 200-250 sccm; and/or the reducing gas and the carbon source are introduced into the reaction chamber at the rates of 120-160 sccm and 60-80 sccm respectively.
9. The method according to claim 1 or 2, characterized in that: the density of the carbon nano tube foam is 0.007-0.009 g/cm3The thickness is 2-2.5 cm.
10. The carbon nanotube foam material with electromagnetic shielding property prepared by the method of any one of claims 1 to 9, which comprises a porous structure consisting of a 3D network structure with self-supporting ability, wherein the porosity of the porous structure is 92 to 96 percent, the pore diameter of pores contained in the porous structure is 10nm to 300 μm, and the density is 0.017 to 0.077g/cm3The thickness of the carbon nanotube foam material is 0.5-5 mm, and the shielding effectiveness of the X wave band is 50-102 dB.
11. Use of the carbon nanotube foam material with electromagnetic shielding property according to claim 10 for preparing electromagnetic shielding material.
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| CN113046024A (en) * | 2021-03-25 | 2021-06-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Shear thickening fluid/carbon nano tube foam impact-resistant energy-absorbing material, preparation method and application |
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