CN111916916B - Carbon nanotube-based three-dimensional network structure composite wave-absorbing material and preparation method thereof - Google Patents
Carbon nanotube-based three-dimensional network structure composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a carbon nanotube-based three-dimensional network structure composite wave-absorbing material and a preparation method thereof, and the wave-absorbing material is characterized by consisting of carbon nanotubes and silicon dioxide, wherein the silicon dioxide is coated on the outer wall of the carbon nanotubes; step 2, ultrasonically dispersing the mixed solution obtained in the step 1; step 3, adjusting the pH value of the mixed solution obtained in the step 2 to 8-10 by using ammonia water; step 4, dropping ethyl orthosilicate into the mixed solution obtained in the step 3, and stirring by using a magnetic stirrer; step 5, respectively filtering the mixed solution obtained in the step 4 by using deionized water and absolute ethyl alcohol; and 6, putting the sample obtained in the step 5 into a drying oven, taking out and grinding the sample into powder to obtain the carbon nanotube-based three-dimensional network structure composite wave-absorbing material. The wave-absorbing material has the advantages of light weight, thin thickness, strong absorption property and the like.
Description
Technical Field
The invention relates to the technical field of structural material preparation, in particular to a carbon nanotube-based three-dimensional network structure composite wave-absorbing material and a preparation method thereof.
Background
It is well known that electromagnetic wave pollution of increasingly serious industrial and domestic electronic equipment is attracting global attention because such pollution is harmful to human health and wildlife. More importantly, the survival of the dominant military forces in war is now critical to the overall battle field. Therefore, in any case, it is critical to design and manufacture an electromagnetic wave absorbing material having high absorption efficiency, wide bandwidth, low density, and good stability under extreme environments.
In recent years, carbon materials have attracted much attention due to their various advantages such as structural diversification and excellent physical and chemical properties. Various carbon materials (carbon black, carbon nanotubes, carbon fibers, graphene, etc.) have been used in aerospace, supercapacitor, and machine manufacturing applications. In addition, the field of electromagnetic wave absorption is also the key field of carbon materials for exerting the advantages of the carbon materials. Among them, carbon nanotubes, which are typical carbon materials, are one of the most widely studied electromagnetic wave absorbing materials due to their excellent specific surface area, low density, and good electrical conductivity absorption performance. Carbon nanotubes have many complimentary inherent properties, such as high specific surface area, low density, high conductivity, etc., and thus can be excellent electromagnetic wave absorbers. However, highly graphitized carbon nanotubes deteriorate impedance matching conditions and produce more electromagnetic wave reflection rather than absorption on the surface thereof. Therefore, the research of the high-efficiency carbon nano tube composite wave-absorbing material has important significance. In conclusion, it is considered that the carbon nanotube-based composite material with excellent impedance matching performance can be prepared by a proper method and can be widely applied to the field of wave absorption.
However, materials conventionally used for compounding with carbon nanotubes are mainly magnetic materials (Fe, Co, Ni, and compounds thereof). These materials have a relatively high density (typically 7-8 g/cm) 3 ). The introduction of these high-density magnetic materials into carbon nanotubes can lead to a substantial increase in the overall density of the composite wave-absorbing material, and may lead to the material being susceptible to corrosion, oxidation or high-temperature failure, so that the advantages of low density, good stability and the like of the carbon nanotubes applied as the wave-absorbing material are no longer obvious, and the designed preparation method and raw materials are also limited. Therefore, it is urgently needed to develop a new preparation method of non-magnetic wave-absorbing material based on carbon nano tube to fill up the defectThis blank space.
Disclosure of Invention
The present invention is to solve the above-mentioned disadvantages of the prior art, and provides a method for introducing silicon dioxide (SiO) while maintaining high dielectric loss of carbon nanotubes 2 ) So as to improve the impedance matching performance of the composite wave-absorbing material and ensure that the prepared three-dimensional reticular carbon nano tube composite material has good wave-absorbing performance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the carbon nanotube-based three-dimensional network structure composite wave-absorbing material is characterized by comprising carbon nanotubes and silicon dioxide, wherein the silicon dioxide is coated on the outer walls of the carbon nanotubes, and the thickness of the silicon dioxide coating is 10-30 nm.
A preparation method of a carbon nanotube-based three-dimensional network structure composite wave-absorbing material is characterized by comprising the following steps:
and step 5, filtering: filtering the mixed solution obtained in the step 4 for 3-6 times by using deionized water and absolute ethyl alcohol respectively;
Preferably, in the step 1, the container is a glass container.
Preferably, in the step 2, the mixed solution is sealed with a plastic film to prevent the ethanol from volatilizing, thereby reducing the dispersion degree, while isolating the external air during the ultrasonic dispersion.
Preferably, in the step 3, ammonia water is used for adjusting the pH value to 9, and the outside air is isolated after the mixing is finished, so that the pH value is prevented from being influenced by the volatilization of the ammonia water.
Preferably, in the step 4, the tetraethoxysilane is dropped into the mixed solution obtained in the step 3, and is stirred for 3 hours by using a magnetic stirrer, wherein in the stirring process, the tetraethoxysilane is firstly stirred at a high speed, the tetraethoxysilane and the carbon nano tube are fully mixed, and then the stirring is carried out at a low speed, so that the formed silicon dioxide coating layer is coated uniformly.
Preferably, in the step 5, the mixture is filtered by deionized water and then filtered by absolute ethyl alcohol, so as to wash away inorganic substances and organic substances which may exist respectively. And the anhydrous ethanol has high volatilization speed and can be dried quickly.
Preferably, in the step 6, the sample obtained in the step 5 is placed in a drying oven and dried for 12 hours at the temperature of 60 ℃.
Preferably, the speed of the rapid stirring is 420-500 r/min, and the speed of the low-speed stirring is 80-120 r/min.
The scheme of the invention has the beneficial effects that: the preparation method of the three-dimensional mesh structure non-magnetic composite wave-absorbing material based on the carbon nano tube is adopted. The carbon nano tube is used as a substrate to ensure high dielectric loss of the composite material, and then the carbon nano tube is mixed with a certain amount of tetraethoxysilane so as to introduce SiO 2 I.e. the production of SiO by sol-gel process 2 And make SiO 2 And growing the coating layer. The obtained carbon nanotube-based three-dimensional network structure composite wave-absorbing material not only retains the excellent performance of the carbon nanotube, but also has good heat resistance and good heat resistance due to the SiO 2 The presence of (a) greatly improves its impedance matching. More importantly, the corrosion resistance, oxidation resistance and high-temperature stability of the material are ensured and avoidedThe harsh reaction conditions required by the high-temperature reaction of the prior method are met. The carbon nanotube-based composite wave-absorbing material prepared by the preparation method has the electromagnetic wave absorption capability which is enhanced by about 120 percent compared with that of a pure carbon nanotube, can be used as an excellent wave-absorbing material with light weight, thin thickness and strong absorption characteristics, and has the advantages of light weight, thin thickness, strong absorption characteristics and the like, so that the material can be used as a more practical wave-absorbing material.
Drawings
Fig. 1 shows XRD patterns of carbon nanotubes before and after SiO2 coating.
Fig. 2 shows a scanning electron micrograph of an original carbon nanotube not coated with SiO2, in which (a) is a low magnification diagram and (b) is a high magnification diagram.
FIG. 3 shows scanning electron microscope spectra of the carbon nanotube composite wave-absorbing material coated with SiO2, wherein (a) is a low-power image and (b) is a high-power image.
Fig. 4 shows a transmission spectrum of the carbon nanotube composite wave-absorbing material coated by SiO2, wherein (a) is a transmission diagram and a selective area electron diffraction pattern diagram of the carbon nanotube coated by SiO2, (b) is a high-resolution transmission diagram of the carbon nanotube coated by SiO2, and (c) and (d) are respectively an element distribution diagram and an element content diagram of the carbon nanotube composite wave-absorbing material coated by SiO 2.
Fig. 5 shows impedance matching patterns of the carbon nanotubes before and after the SiO2 coating.
Fig. 6 shows reflection losses of the carbon nanotubes before and after coating with SiO2, where (a) is a reflection loss graph of the carbon nanotubes without SiO2 coating at different thicknesses, and (b) is a reflection loss graph of the carbon nanotubes coated with SiO2 at different thicknesses.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
as shown in the attached drawing, the carbon nanotube-based three-dimensional network structure composite wave-absorbing material is characterized in that the adsorbing material is composed of carbon nanotubes and silicon dioxide, the silicon dioxide is coated on the outer walls of the carbon nanotubes, and the thickness of the silicon dioxide coating is 10-30 nm.
A preparation method of a carbon nanotube-based three-dimensional network structure composite wave-absorbing material is characterized by comprising the following steps:
and step 5, filtering: filtering the mixed solution obtained in the step 4 for 3-6 times by using deionized water and absolute ethyl alcohol respectively;
Preferably, in the step 1, the container is a glass container.
Preferably, in the step 2, the mixed solution is sealed with a plastic film to prevent the ethanol from volatilizing, thereby reducing the dispersion degree, while isolating the external air during the ultrasonic dispersion.
Preferably, in the step 3, ammonia water is used for adjusting the pH value to 9, and the outside air is isolated after the mixing is finished, so that the pH value is prevented from being influenced by the volatilization of the ammonia water.
Preferably, in the step 4, the tetraethoxysilane is dropped into the mixed solution obtained in the step 3, and is stirred for 3 hours by using a magnetic stirrer, wherein in the stirring process, the tetraethoxysilane is firstly stirred at a high speed, the tetraethoxysilane and the carbon nano tube are fully mixed, and then the stirring is carried out at a low speed, so that the formed silicon dioxide coating layer is coated uniformly.
Preferably, in the step 5, the mixture is filtered by deionized water and then filtered by absolute ethyl alcohol, so as to wash away inorganic substances and organic substances which may exist respectively. And the anhydrous ethanol has high volatilization speed and can be dried quickly.
Preferably, in the step 6, the sample obtained in the step 5 is placed in a drying oven and dried for 12 hours at the temperature of 60 ℃.
Preferably, the speed of the rapid stirring is 420-500 r/min, and the speed of the low-speed stirring is 80-120 r/min.
The process for introducing the carbon source into the tetraethoxysilane comprises the following steps:
the product according to the scheme is contrastively analyzed with the prior art, and the performance of the product according to the scheme is as follows:
as shown in FIG. 1: FIG. 1 shows XRD patterns of carbon nanotubes before and after coating with SiO2, wherein Sample A is the XRD pattern of the original carbon nanotube which is not coated with SiO2, and Sample B is the XRD pattern of the carbon nanotube composite wave-absorbing material coated with SiO 2;
as shown in FIG. 1, a comparison of Sample A and Sample B reveals that SiO is responsible for 2 The existence of the coating layer weakens the XRD diffraction peak of the carbon nano tube, and reflects the success of SiO2 coating from one side surface.
As shown in fig. 2: fig. 2 shows a scanning electron micrograph of an original carbon nanotube not coated with SiO2, in which (a) is a low magnification diagram and (b) is a high magnification diagram. The carbon nano tube without the SiO2 coating is exposed and relatively smooth;
as shown in fig. 3: fig. 3 shows a scanning electron microscope atlas of the carbon nanotube composite wave-absorbing material coated with SiO2, where fig. 3 (a) is a low-power image and fig. 3 (b) is a high-power image.
It can be seen from the comparison between fig. 2 and fig. 3 that the SiO 2-coated carbon nanotubes form aggregates on the surface, which are relatively rough, and thus may generate more interface loss, thereby improving the wave-absorbing performance.
As shown in FIG. 4: fig. 4 shows a transmission spectrum of a carbon nanotube composite wave-absorbing material coated with SiO2, where fig. 4 (a) is a transmission diagram and a selected area electron diffraction pattern diagram of a carbon nanotube coated with SiO2, fig. 4 (b) is a high-resolution transmission diagram of a carbon nanotube coated with SiO2, fig. 4 (C) and fig. 4(d) are element distribution and element content diagrams of a carbon nanotube composite wave-absorbing material coated with SiO2, respectively, it is apparent from fig. 4 (a) that a layer of coating is on the surface of a carbon nanotube and the coating layer is amorphous, from fig. 4 (b), the thickness of the coating layer is 17.98-18.23 nm, from fig. 4 (C), and from fig. 4(d), the elements forming the composite are C, O, and Si, and the content of each element is shown in fig. 4(d), and it can be determined that the method can coat a layer of SiO2 on the surface of a carbon nanotube.
As shown in FIG. 5: FIG. 5 shows the impedance matching patterns of the carbon nanotubes before and after SiO2 coating, wherein Sample A is the impedance matching pattern of the original carbon nanotube which is not coated by SiO2, Sample B is the impedance matching pattern of the carbon nanotube composite wave-absorbing material coated by SiO2,
it can be seen that the impedance matching value of Sample B is far better than that of Sample A, the impedance matching performance and the wave-absorbing performance are in positive correlation, and 1 is the optimal impedance matching, so that the impedance matching value of the product reaches 0.99 at 14GHz, and is basically the optimal value.
As shown in fig. 6: FIG. 6 shows reflection loss of carbon nanotubes with different thicknesses before and after coating with SiO2, where FIG. 6(a) is a reflection loss graph of carbon nanotubes without SiO2 coating with different thicknesses, and FIG. 6(b) is a reflection loss graph of carbon nanotubes with different thicknesses after coating with SiO2
Fig. 6(a) shows that the reflection loss of the carbon nanotube is far less than-10 dB (the reflection loss can be practically applied only when the reflection loss reaches-10 dB), fig. 6(b) shows that the reflection loss of the carbon nanotube coated with Si02 is as high as-54.076 dB (reaches 99.999% of electromagnetic wave absorption rate) under the thickness of 1.08mm, and compared with the carbon nanotube which is not coated, the wave absorbing performance is improved by about 120%, so that the wave absorbing performance of the carbon nanotube coated with the silicon carbide composite material is better.
In addition, the prior art also adopts the prior art of directly combining silicon dioxide and carbon nano tubes with composite materials, but in the prior art, silicon dioxide crystals are directly mixed with the carbon nano tubes, and different from the patent that tetraethoxysilane is adopted as a silicon source to generate SiO2, the direct adoption of silicon dioxide has to be subjected to steps of rolling, high temperature and the like, and the processing cost is higher. The composite material of the carbon nano tube coated by SiO2 can be generated at normal temperature and normal pressure by adopting tetraethoxysilane as a silicon source.
The loading amount and the temperature of the carbon nano tube of the composite material adopting the direct mixing of the silicon dioxide crystal and the carbon nano tube have great influence on the performance of the composite material, and under the manufacturing condition of 100 ℃ and 500 ℃, the reflection loss is only less than-7 dB when the carbon nano tube is loaded to 2 wt% (under the normal-temperature manufacturing condition, when the carbon nano tube is loaded to 0.4-0.6 wt%, the reflection loss exceeds-10 dB under any thickness of 1-5.5 mm). When the carbon nano tube load reaches 5 wt.%, the reflection loss is greatly improved.
In addition, in this patent, the performance of coating structure compares with the material of mixed silica, the coating structure mainly uses carbon nanotube as the base, can give full play to the excellent performance of carbon nanotube, and use SiO2 microballon as the base among the prior art, the load capacity of carbon nanotube is only 2~10%, SiO2 content can cause the density of combined material to increase (SiO2 density is 2.2g/cm year, carbon nanotube density is 1.3~ 2g/cm year), be unfavorable for absorbing the practical application of material.
The scheme of the invention has the beneficial effect of adopting the preparation method of the carbon nanotube-based three-dimensional network structure composite wave-absorbing material. The carbon nano tube is used as a substrate to ensure the high dielectric loss and the high electromagnetic wave absorption performance of the composite material, and then the carbon nano tube is mixed with a certain amount of tetraethoxysilane to introduce SiO 2 I.e. the production of SiO by sol-gel processes 2 And make SiO 2 And growing the coating layer. The obtained non-magnetic composite wave-absorbing material with the three-dimensional network structure based on the carbon nano tube not only keeps the excellent performance of the carbon nano tube, but also has the advantages of good performance and low cost due to the SiO 2 The presence of (a) greatly improves its impedance matching. More importantly, the corrosion resistance, oxidation resistance and high-temperature stability of the material are ensured, and the harsh reaction conditions required by the high-temperature reaction of the prior method are avoided. These advantages make the material a more practical wave-absorbing material.
Claims (8)
1. A preparation method of a carbon nanotube-based three-dimensional network structure composite wave-absorbing material is characterized in that the wave-absorbing material is composed of carbon nanotubes and silicon dioxide, the silicon dioxide is coated on the outer walls of the carbon nanotubes, the thickness of the silicon dioxide coating is 10-30 nm, and the preparation method comprises the following steps:
step 1, mixing materials: mixing absolute ethyl alcohol and deionized water to obtain a mixed solution, wherein the mass percent of the absolute ethyl alcohol is 40-50% of that of the deionized water, putting the mixed solution of the absolute ethyl alcohol and the deionized water into a container, and adding carbon nano tubes into the mixed solution, wherein the mass percent of the carbon nano tubes is 0.4-0.6% of that of the mixed solution;
Step 2, dispersing: ultrasonically dispersing the mixed solution containing the carbon nano tubes obtained in the step 1 for 2-4 h;
step 3, pH value blending: adjusting the pH value of the mixed solution obtained in the step 2 to 8-10 by using ammonia water;
step 4, coating: dropping ethyl orthosilicate into the mixed solution obtained in the step 3, and stirring by using a magnetic stirrer, wherein the mass percent of the ethyl orthosilicate is 0.8-1% of the mixed solution obtained in the step 3;
and step 5, filtering: filtering the mixed solution obtained in the step 4 for 3-6 times by using deionized water and absolute ethyl alcohol respectively;
step 6, drying and grinding: and (4) putting the sample obtained in the step (5) into a drying oven, drying for 12-14 h at the temperature of 60 ℃, taking out, and grinding into powder to obtain the carbon nanotube-based three-dimensional network structure composite wave-absorbing material.
2. The method for preparing the carbon nanotube-based three-dimensional network structure composite wave-absorbing material as claimed in claim 1, wherein in the step 1, the container is a glass container.
3. The method for preparing the composite wave-absorbing material with the carbon nanotube-based three-dimensional network structure as claimed in claim 1, wherein in the step 2, the mixed solution is sealed by a plastic film while being isolated from the outside air during the ultrasonic dispersion.
4. The method for preparing the carbon nanotube-based three-dimensional network structure composite wave-absorbing material according to claim 1, wherein in the step 3, ammonia water is used for adjusting the pH value to 9, and the outside air is isolated after the mixing.
5. The method for preparing the carbon nanotube-based three-dimensional network structure composite wave-absorbing material as claimed in claim 1, wherein in the step 4, tetraethoxysilane is dropped into the mixed solution obtained in the step 3, and is stirred for 3 hours by a magnetic stirrer, wherein in the stirring process, the tetraethoxysilane and the carbon nanotube are firstly stirred rapidly, and are fully mixed, and then are stirred slowly, so that the formed silicon dioxide coating layer is coated uniformly.
6. The method for preparing the carbon nanotube-based three-dimensional network structure composite wave-absorbing material as claimed in claim 1, wherein in the step 5, the filtering is performed with deionized water and then with absolute ethyl alcohol.
7. The method for preparing the carbon nanotube-based three-dimensional network structure composite wave-absorbing material according to claim 1, wherein the sample obtained in the step 5 is placed in a drying oven and dried for 12 hours at 60 ℃ in the step 6.
8. The method for preparing a carbon nanotube-based three-dimensional network composite wave-absorbing material as claimed in claim 5, wherein the rapid stirring speed is 420-500 r/min, and the slow stirring speed is 80-120 r/min.
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| CN114447621A (en) * | 2021-12-22 | 2022-05-06 | 山东大学 | Composite hollow fiber wave-absorbing material and preparation method and application thereof |
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