CN111205819A - Carbon nanotube-aluminum nitride wave absorbing agent and preparation method thereof, carbon nanotube-aluminum nitride composite wave absorbing material and application thereof - Google Patents
Carbon nanotube-aluminum nitride wave absorbing agent and preparation method thereof, carbon nanotube-aluminum nitride composite wave absorbing material and application thereof Download PDFInfo
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Abstract
The invention provides a carbon nano tube-aluminum nitride wave absorbing agent and a preparation method thereof, a carbon nano tube-aluminum nitride composite wave absorbing material and application thereof, and belongs to the technical field of wave absorbing materials. The carbon nano tube-aluminum nitride wave absorbing agent provided by the invention comprises a carbon nano tube and aluminum nitride; the aluminum nitride is coated on the surface of the carbon nano tube; the length of the carbon nanotube is 2-10 mu m; the mass of the carbon nano tube accounts for 1-10% of the total mass of the carbon nano tube-aluminum nitride wave absorber. The aluminum nitride adopted by the invention has good thermal shock resistance, dielectric property and molten metal corrosion resistance; the carbon nano tube has the excellent characteristics of large specific surface area, high aspect ratio, excellent mechanical strength, outstanding dielectric property and the like, and meanwhile, functional groups or chemical bonds on the surface of the carbon nano tube are replaced or combined with chemical bonds in the aluminum nitride, so that the dispersibility of the carbon nano tube in the carbon nano tube-aluminum nitride wave absorbing agent is improved, and the wave absorbing property of the carbon nano tube-aluminum nitride wave absorbing agent is excellent.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a carbon nano tube-aluminum nitride wave-absorbing agent and a preparation method thereof, a carbon nano tube-aluminum nitride composite wave-absorbing material and application thereof.
Background
With the rapid development of modern technological progress and the development of electronic information technology in the civil field, the derived electromagnetic wave radiation causes many complex problems such as electromagnetic pollution, electromagnetic interference, information disclosure and the like, and the development of the fields such as the information industry, the electronic industry and the like is hindered; for national defense construction, particularly, the microwave electronic technology and the advanced radar are taken as effective means for improving the survival, penetration and depth capabilities of weapon systems, and the microwave electronic technology and the advanced radar are one of the hot spots in the world of the strong military and the country corner-to-corner military and the advanced field. Therefore, the development of a material capable of absorbing electromagnetic waves in a specific frequency band is an effective means for solving the problems at present, and has high research value and application prospect.
The wave-absorbing material can absorb or greatly weaken the electromagnetic wave energy projected to the surface of the wave-absorbing material as an important electromagnetic wave material, reduce the electromagnetic wave interference, convert the loss of the material into heat energy, and greatly ensure the health of human beings and reduce the harm brought by electromagnetism when being applied to the civil field; in the field of national defense construction, the influence of detection systems such as radar and infrared on a target can be weakened as much as possible, and the penetration, attack and survival capability of a weapon system or an aircraft can be obviously improved. Carbon Nanotubes (CNTs), an important novel one-dimensional nanomaterial, have excellent properties such as a large specific surface area, a high aspect ratio, excellent mechanical strength, and outstanding dielectric properties, and have attracted much attention in the field of electromagnetic wave material absorption. However, the carbon nanotubes have small tube diameter and large surface energy, and are very easy to tangle and agglomerate together, which seriously affects the uniform dispersion of the carbon nanotubes in the polymer, so that the wave-absorbing performance of the wave-absorbing material is affected to a certain extent.
Disclosure of Invention
In view of the above, the present invention provides a carbon nanotube-aluminum nitride wave-absorbing agent, a preparation method thereof, a carbon nanotube-aluminum nitride composite wave-absorbing material, and applications thereof. The carbon nanotube-aluminum nitride wave absorber provided by the invention has good dispersibility of the carbon nanotube and excellent wave absorbing performance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a carbon nano tube-aluminum nitride wave absorbing agent, which comprises a carbon nano tube and aluminum nitride; the aluminum nitride is coated on the surface of the carbon nano tube;
the mass of the carbon nano tube accounts for 1-10% of the total mass of the carbon nano tube-aluminum nitride wave absorber;
preferably, the outer diameter of the carbon nanotube is 30-50 nm in length; the length of the carbon nanotube is 2-10 mu m.
Preferably, the aluminum nitride is needle-shaped, the length of the aluminum nitride is 60-120 nm, and the diameter of the aluminum nitride is 5-15 nm.
The invention provides a preparation method of the carbon nano tube-aluminum nitride wave absorbing agent in the technical scheme, which comprises the following steps:
mixing the carbon nano tube, the aluminum nitride and the anhydrous dispersant, and carrying out modification treatment to obtain the carbon nano tube-aluminum nitride wave absorber.
Preferably, the mixing is ultrasonic dispersion; the ultrasonic dispersion time is 60-180 min.
Preferably, the temperature of the modification treatment is 80-160 ℃, the time is 4-10 h, and the rate of heating to the modification treatment temperature is 2-4 ℃/min.
Preferably, the anhydrous dispersant comprises anhydrous N, N-dimethylformamide or anhydrous ethanol.
The invention provides a carbon nano tube-aluminum nitride composite wave-absorbing material, which comprises a carbon nano tube-aluminum nitride wave-absorbing agent and paraffin;
the carbon nanotube-aluminum nitride wave absorber is the carbon nanotube-aluminum nitride wave absorber in the technical scheme or the carbon nanotube-aluminum nitride wave absorber prepared by the preparation method in the technical scheme.
Preferably, the mass ratio of the carbon nanotube-aluminum nitride wave absorber to the paraffin is 1: 9-2: 3.
The invention also provides the application of the carbon nano tube-aluminum nitride composite wave-absorbing material in the technical scheme in a thermosensitive element, a photosensitive element, an electronic element, an intelligent element or a sensor.
The invention provides a carbon nano tube-aluminum nitride wave absorbing agent, which comprises a carbon nano tube and aluminum nitride; the aluminum nitride is coated on the surface of the carbon nano tube; the mass of the carbon nano tube accounts for 1-10% of the total mass of the carbon nano tube-aluminum nitride wave absorber. The aluminum nitride (ALN) adopted by the invention has good thermal shock resistance, dielectric property and molten metal corrosion resistance; the Carbon Nano Tubes (CNTs) have the excellent characteristics of large specific surface area, high aspect ratio, excellent mechanical strength, outstanding dielectric property and the like, the carbon nano tubes can avoid serious agglomeration phenomenon by adopting specific content, the dispersibility of the carbon nano tubes in aluminum nitride is improved, and meanwhile, the wave absorbing performance of the carbon nano tube-aluminum nitride wave absorbing agent is excellent; the length of the carbon nano tube also has influence on agglomeration, and overlength can cause mutual winding, bending and even length recombination among a plurality of carbon tubes, and the mutual winding, bending and even length recombination have interference effects on the formation of the morphology of the carbon nano tube-aluminum nitride wave absorbing agent and the stability of the final wave absorbing performance; meanwhile, functional groups or chemical bonds on the surface of the carbon nano tube-aluminum nitride wave absorber are replaced or combined with chemical bonds in the aluminum nitride, so that the prepared carbon nano tube-aluminum nitride wave absorber has excellent wave absorbing performance.
The preparation method of the carbon nano tube-aluminum nitride wave absorber provided by the invention is simple to operate and suitable for industrial production.
The carbon nanotube-aluminum nitride composite wave-absorbing material provided by the invention is small in using amount, wide in effective absorption frequency band in reflection loss, large in reflection loss and excellent in wave-absorbing performance. As shown by the results of the embodiment of the invention, the real part of the dielectric constant of the carbon nanotube-aluminum nitride composite wave-absorbing material is 3.18-17.60; the imaginary part is 0.36-12.94; the real part of the magnetic conductivity is 0.83-1.12; the imaginary part of the magnetic conductivity is 0.05-0.54; the reflection loss is-4.93 to-50 dB; the wave-absorbing bandwidth is 2-18 GHz; the thickness of the material is 0.1-6 mm.
Drawings
FIG. 1 is an SEM image of carbon nanotube-aluminum nitride absorbents prepared in examples 1-4 and comparative example 1, wherein (a) is example 1, (b) is example 2, (c) is example 3, (d) is example 4, and (e) is comparative example 1;
FIG. 2 is an XRD plot of aluminum nitride (ALN), carbon nanotubes (MWCNTs) and the carbon nanotube-aluminum nitride absorber prepared in example 3;
FIG. 3 is an infrared spectrum of the carbon nanotube-aluminum nitride absorber prepared in examples 1 to 4;
fig. 4 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in example 5, in which (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
fig. 5 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in example 6, in which (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
fig. 6 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in example 7, in which (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
fig. 7 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in example 8, in which (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
FIG. 8 is a reflection loss chart of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in comparative example 2, in which (a) is a reflection loss 3D chart, and (b) is a reflection loss 2D chart;
fig. 9 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in example 9, in which (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
fig. 10 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in example 10, in which (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
FIG. 11 is a reflection loss diagram of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in comparative example 3, wherein (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram;
FIG. 12 is a graph showing the variation of dielectric constant and permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 11-14 in the range of 2-18 GHz, wherein (a) is the real part of the dielectric constant, (b) is the imaginary part of the dielectric constant, (c) is the real part of the permeability, and (d) is the imaginary part of the permeability;
fig. 13 is a graph showing the variation of the dielectric constant and the permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 15 to 18 in the range of 2 to 18GHz, wherein (a) is a real part of the dielectric constant, (b) is an imaginary part of the dielectric constant, (c) is a real part of the permeability, and (d) is an imaginary part of the permeability;
FIG. 14 is a graph showing the variation of dielectric constant and permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 19 to 22 in the range of 2 to 18GHz, wherein (a) is the real part of the dielectric constant, (b) is the imaginary part of the dielectric constant, (c) is the real part of the permeability, and (d) is the imaginary part of the permeability;
fig. 15 is a graph showing the variation of the dielectric constant and the magnetic permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 23 to 26 in the range of 2 to 18GHz, wherein (a) is a real part of the dielectric constant, (b) is an imaginary part of the dielectric constant, (c) is a real part of the magnetic permeability, and (d) is an imaginary part of the magnetic permeability.
Detailed Description
The invention provides a carbon nano tube-aluminum nitride wave absorbing agent, which comprises a carbon nano tube and aluminum nitride; the aluminum nitride is coated on the surface of the carbon nano tube;
the mass of the carbon nano tube accounts for 1-10% of the total mass of the carbon nano tube-aluminum nitride wave absorber.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
In the present invention, the carbon nanotube is preferably a single-walled carbon nanotube or a multi-walled carbon nanotube. In the invention, the length of the carbon nanotube is preferably 2-10 μm, more preferably 3-9 μm, more preferably 4-8 μm, and most preferably 4-6 μm; the outer diameter of the carbon nano tube is preferably 30-50 nm, more preferably 35-45 nm, and most preferably 40-45 nm; the wall thickness of the carbon nano tube is preferably 0.05-0.07 nm, and more preferably 0.06 nm. In the invention, the carbon nanotube with too small length is not beneficial to synthesizing the carbon nanotube-aluminum nitride wave absorbing agent with aluminum nitride, and can cause adverse effect on the stability of the structure of the carbon nanotube-aluminum nitride wave absorbing agent, thereby further influencing the wave absorbing performance of the carbon nanotube-aluminum nitride wave absorbing agent. The invention can further improve the wave absorbing performance of the carbon nano tube-aluminum nitride wave absorbing agent by adopting the carbon nano tube with the specific length. In the present invention, the carbon nanotubes are preferably purchased from Nanjing Xiancheng nanomaterial science and technology Co.
In the invention, the aluminum nitride is preferably needle-shaped, and the length of the aluminum nitride is preferably 60-120 nm, more preferably 70-110 nm, and most preferably 80-100 nm; the diameter of the aluminum nitride is preferably 5-15 nm, more preferably 7-12 nm, and most preferably 10-12 nm. In the present invention, the aluminum nitride is preferably purchased from Shanghai ultra Wen nanotechnology, Inc.
In the present invention, the mass of the carbon nanotube is preferably 2 to 9%, more preferably 3 to 8%, and most preferably 5 to 7% of the total mass of the carbon nanotube and the aluminum nitride.
The aluminum nitride (ALN) adopted by the invention has good thermal shock resistance, dielectric property and molten metal corrosion resistance; the Carbon Nano Tubes (CNTs) have the excellent characteristics of large specific surface area, high aspect ratio, excellent mechanical strength, outstanding dielectric property and the like, functional groups or chemical bonds (oxygen-containing functional groups such as carbon-carbon bonds, hydroxyl groups and the like) on the surfaces of the carbon nano tubes are substituted or combined with chemical bonds in aluminum nitride, the dispersity of the carbon nano tubes in the carbon nano tube-aluminum nitride wave absorber is improved, and the wave absorbing performance of the carbon nano tube-aluminum nitride wave absorber is excellent.
The invention provides a preparation method of the carbon nano tube-aluminum nitride wave absorbing agent in the technical scheme, which comprises the following steps:
mixing the carbon nano tube, the aluminum nitride and the anhydrous dispersant, and carrying out modification treatment to obtain the carbon nano tube-aluminum nitride wave absorber.
In the present invention, the anhydrous dispersant preferably includes N, N-dimethylformamide or anhydrous ethanol, and more preferably N, N-dimethylformamide. In the invention, the aluminum nitride is easy to generate hydrolysis reaction with water, and the anhydrous dispersant is used as the anhydrous dispersant, so that the side reaction of the aluminum nitride can be avoided, and the wave absorbing performance of the carbon nano tube-aluminum nitride wave absorbing agent is improved. In the present invention, the ratio of the mass of the carbon nanotube to the volume of the anhydrous dispersant is preferably 1 g: (2-4) L, more preferably 1 g: (2-3) L.
In the present invention, the mixing is preferably ultrasonic dispersion; the temperature of the ultrasonic dispersion is preferably 5-40 ℃, and more preferably 10-35 ℃; in the embodiments of the present invention, the ultrasonic dispersion is preferably performed under room temperature conditions; the time for ultrasonic dispersion is preferably 60-180 min, more preferably 80-160 min, and most preferably 90-150 min. The invention adopts ultrasonic dispersion to enable the carbon nano tube and the aluminum nitride to be dispersed in the anhydrous dispersant more uniformly.
In the invention, the temperature of the modification treatment is preferably 80-160 ℃, more preferably 90-150 ℃, and most preferably 100-120 ℃; the time of the modification treatment is preferably 4-10 h, more preferably 5-8 h, and most preferably 6-7 h; the rate of raising the temperature to the modification treatment temperature is preferably 2 to 4 ℃/min, more preferably 3 ℃/min, and most preferably 3.5 ℃/min. In the present invention, the modification treatment is preferably performed under oil bath conditions.
In the present invention, in order to avoid gas volatilization of the anhydrous dispersant caused by an excessively high temperature during the temperature rise of the oil bath during the modification treatment, it is preferable to add a condensation tube to the reaction vessel side to perform condensation or reflux. In the invention, functional groups or chemical bonds on the surface of the carbon nano tube are replaced or combined with chemical bonds in the aluminum nitride in the modification treatment process, so that the dispersibility and the wave absorbing performance of the carbon nano tube in the carbon nano tube-aluminum nitride wave absorbing agent are improved.
After the modification treatment, the invention preferably further comprises the steps of cooling the wave absorbing agent reaction system obtained by the modification treatment to room temperature, carrying out solid-liquid separation, washing and drying to obtain the carbon nano tube-aluminum nitride wave absorbing agent. The cooling method of the present invention is not particularly limited, and a cooling method known in the art may be used; in an embodiment of the invention, the cooling is preferably natural cooling. The solid-liquid separation mode is not particularly limited, and a solid-liquid separation mode well known in the field can be adopted; in the embodiment of the present invention, the solid-liquid separation method is preferably suction filtration. In the present invention, the washing preferably includes an absolute ethanol washing and an ultrapure water washing performed in this order, and the number of times of the absolute ethanol washing and the ultrapure water washing is not particularly limited, and the pH of the solution after washing may be close to 7. The drying mode is not particularly limited in the invention, and the drying mode known in the field can be adopted; in the embodiment of the present invention, the drying manner is preferably drying. In the invention, the drying temperature is preferably 55-85 ℃, and more preferably 60-80 ℃; the drying time is preferably 12-24 hours, and more preferably 15-21 hours.
The preparation method provided by the invention is simple to operate and suitable for industrial production. And the carbon nano-tube can not be agglomerated in the preparation process; the obtained carbon nano tube-aluminum nitride wave absorbing agent has excellent wave absorbing performance.
The invention provides a carbon nano tube-aluminum nitride composite wave-absorbing material, which comprises a carbon nano tube-aluminum nitride wave-absorbing agent and paraffin;
the carbon nanotube-aluminum nitride wave absorber is the carbon nanotube-aluminum nitride wave absorber in the technical scheme or the carbon nanotube-aluminum nitride wave absorber prepared by the preparation method in the technical scheme.
In the invention, the mass ratio of the carbon nanotube-aluminum nitride wave absorber to the paraffin is preferably 1:9 to 2:3, and more preferably 1:4 to 3: 7.
In the carbon nanotube-aluminum nitride composite wave-absorbing material, the mass percentage of the paraffin is preferably 60-90%, more preferably 65-85%, and most preferably 70-80%.
In the invention, the thickness of the carbon nanotube-aluminum nitride composite wave-absorbing material is preferably 0.1-6 mm, more preferably 0.5-5.5 mm, and most preferably 1-5 mm.
The carbon nanotube-aluminum nitride composite wave-absorbing material provided by the invention is small in thickness, large in reflection loss, wide in wave-absorbing bandwidth range and excellent in wave-absorbing performance when in use.
In the invention, the preparation method of the carbon nanotube-aluminum nitride composite wave-absorbing material preferably comprises the following steps: mixing the carbon nano tube-aluminum nitride wave absorbing agent with paraffin to obtain mixed powder; and carrying out compression ring on the mixed powder to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The mixing method of the present invention is not particularly limited, and a mixing method known in the art may be used. In the invention, the pressing ring is preferably carried out by placing the mixed powder in a pressing ring mold. The size of the pressing ring mold is not particularly limited, and the pressing ring mold known in the field can be adopted. In an embodiment of the present invention, the size of the pressing ring mold is preferably: the inner diameter is 3.04mm, the outer diameter is 7.00mm, and the size of the obtained carbon nano tube-aluminum nitride composite wave-absorbing material is consistent with that of a mould.
The invention also provides the application of the carbon nano tube-aluminum nitride composite wave-absorbing material in the technical scheme in a thermosensitive element, a photosensitive element, an electronic element, an intelligent element or a sensor.
In the present invention, the field of application preferably includes the defense industry, the optical field, the medical field, the battery field, or the material field.
In the invention, the carbon nano tube-aluminum nitride composite wave-absorbing material has the function of converting measured external information into electric signals or other information in a required form according to a certain rule for re-reaction and output so as to meet the requirements on information transmission, processing, display, control and the like; or the electromagnetic wave energy projected to the surface of the material is absorbed or weakened to the maximum extent, so that the interference of the electromagnetic wave to bodies of aircrafts and the like is reduced to the minimum extent, and the survival and the anti-attack capability of the bodies are improved.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 300mL of DMF (dimethyl formamide) into a beaker with the capacity of 500mL, adding 20mg of multi-walled carbon nanotubes (MWCNTs, the length is 5-8 mu m mostly, the diameter is 30-35 nm, and the wall thickness is about 0.06nm) and 0.98g of aluminum nitride, and placing the beaker into an ultrasonic machine for ultrasonic dispersion for 1h to obtain a mixed solution; transferring the mixed solution into a round-bottom flask, adding a magneton, adding a condenser pipe on one side of the round-bottom flask, fixing the experimental device in an oil bath device, starting modification treatment, heating to 130 ℃ at a heating rate of 3.5 ℃/min under the condition of magnetic stirring, and carrying out modification reaction for 9 hours. After the reaction is finished, naturally cooling the whole experimental device to room temperature, and taking out the round-bottom flask; carrying out suction filtration on the obtained wave absorbing agent solution to obtain a solid; and (2) sequentially washing the solid with absolute ethyl alcohol and ultrapure water, and then drying in an oven at 70 ℃ for 24 hours to obtain the carbon nanotube-aluminum nitride wave absorber (abbreviated as ALN @ 2% MWCNTs).
Example 2
Adding 300mL of DMF (dimethyl formamide) into a beaker with the capacity of 500mL, adding 100mg of multi-wall carbon nano tubes (the length is 5-8 mu m mostly, the diameter is 30-35 nm, and the wall thickness is about 0.06nm) and 1.9g of aluminum nitride, and placing the beaker into an ultrasonic machine for ultrasonic dispersion for 1.5h to obtain a mixed solution; transferring the mixed solution into a round-bottom flask, adding a magneton, adding a condenser pipe on one side of the round-bottom flask, fixing the experimental device in an oil bath device, starting an oil bath experiment, heating to 120 ℃ at a heating rate of 3.5 ℃/min under the condition of magnetic stirring, and reacting for 8 hours. After the reaction is finished, naturally cooling the whole experimental device to room temperature, and taking out the round-bottom flask; carrying out suction filtration on the obtained wave absorbing agent solution to obtain a solid; and (2) sequentially washing the solid with absolute ethyl alcohol and ultrapure water, and then drying in an oven at 70 ℃ for 24 hours to obtain the carbon nanotube-aluminum nitride wave absorber (abbreviated as ALN @ 5% MWCNTs).
Example 3
Adding 300mL of DMF (dimethyl formamide) into a beaker with the capacity of 500mL, adding 140mg of multi-wall carbon nano tubes (the length is 5-8 mu m mostly, the diameter is 30-35 nm, and the wall thickness is about 0.06nm) and 1.86g of aluminum nitride, and placing the beaker into an ultrasonic machine for ultrasonic dispersion for 1h to obtain a mixed solution; transferring the mixed solution into a round-bottom flask, adding a magneton, adding a condenser pipe on one side of the round-bottom flask, fixing the experimental device in an oil bath device, starting an oil bath experiment, heating to 120 ℃ at a heating rate of 3.5 ℃/min under the condition of magnetic stirring, and reacting for 8 hours. After the reaction is finished, naturally cooling the whole experimental device to room temperature, and taking out the round-bottom flask; carrying out suction filtration on the obtained wave absorbing agent solution to obtain a solid; and (2) sequentially washing the solid with absolute ethyl alcohol and ultrapure water, and then drying in an oven at 70 ℃ for 24 hours to obtain the carbon nanotube-aluminum nitride wave absorber (abbreviated as ALN @ 7% MWCNTs).
Example 4
Adding 300mL of DMF (dimethyl formamide) into a beaker with the capacity of 500mL, adding 100mg of multi-wall carbon nano tubes (the length is 5-8 mu m mostly, the diameter is 30-35 nm, and the wall thickness is about 0.06nm) and 0.9g of aluminum nitride, and placing the beaker into an ultrasonic machine for ultrasonic dispersion for 1h to obtain a mixed solution; transferring the mixed solution into a round-bottom flask, adding a magneton, adding a condenser pipe on one side of the round-bottom flask, fixing the experimental device in an oil bath device, starting an oil bath experiment, heating to 100 ℃ at a heating rate of 3.5 ℃/min under the condition of magnetic stirring, and reacting for 9 hours. After the reaction is finished, naturally cooling the whole experimental device to room temperature, and taking out the round-bottom flask; carrying out suction filtration on the obtained wave absorbing agent solution to obtain a solid; and (2) sequentially washing the solid with absolute ethyl alcohol and ultrapure water, and then drying in an oven at 60 ℃ for 24 hours to obtain the carbon nanotube-aluminum nitride wave absorber (abbreviated as ALN @ 10% MWCNTs).
Comparative example 1
Adding 300mL of DMF (dimethyl formamide) into a beaker with the capacity of 500mL, adding 150mg of carbon nanotubes (the length is 5-8 mu m mostly, the diameter is 30-35 nm, and the wall thickness is about 0.06nm) and 0.85g of aluminum nitride, and placing the beaker into an ultrasonic machine for ultrasonic dispersion for 1 hour to obtain a mixed solution; transferring the mixed solution into a round-bottom flask, adding a magneton, adding a condenser pipe on one side of the round-bottom flask, fixing the experimental device in an oil bath device, starting an oil bath experiment, heating to 100 ℃ at a heating rate of 3.5 ℃/min under the condition of magnetic stirring, and reacting for 9 hours. After the reaction is finished, naturally cooling the whole experimental device to room temperature, and taking out the round-bottom flask; carrying out suction filtration on the obtained wave absorbing agent solution to obtain a solid; and (2) sequentially washing the solid with absolute ethyl alcohol and ultrapure water, and then drying in an oven at 60 ℃ for 24 hours to obtain the carbon nanotube-aluminum nitride wave absorber (abbreviated as ALN @ 15% MWCNTs).
SEM images of the carbon nanotube-aluminum nitride wave absorbers prepared in examples 1-4 and comparative example 1 are shown in FIG. 1, wherein (a) is example 1, (b) is example 2, (c) is example 3, (d) is example 4, and (e) is comparative example 1. As can be seen from fig. 1, when the content of the carbon nanotubes is too low, the aluminum nitride cannot be sufficiently bonded with the carbon nanotubes, and the dispersibility between the aluminum nitride and the carbon nanotubes is poor, so that serious agglomeration occurs, whereas when the content of the carbon nanotubes is 7%, the synthesized material has the best morphology, the aluminum nitride can be uniformly distributed on the surfaces of the carbon nanotubes to modify the surfaces, and when the content of the carbon nanotubes is 15%, the carbon nanotubes are seriously agglomerated. The reason is that the content of the carbon nano tube is too large, so that the aluminum nitride cannot be sufficiently compounded with the carbon nano tube, and more carbon nano tubes generate a serious agglomeration phenomenon, so that the wave absorbing performance of the carbon nano tube-aluminum nitride wave absorbing agent is inhibited.
The infrared spectra of aluminum nitride (ALN), carbon nanotubes (MWCNTs), and the carbon nanotube-aluminum nitride absorber prepared in example 3 are shown in fig. 2. As can be seen from fig. 2, the carbon nanotube-aluminum nitride absorber was successfully prepared by comparing the infrared spectra of the carbon nanotube, aluminum nitride and the carbon nanotube-aluminum nitride absorber.
XRD of the carbon nanotube-aluminum nitride absorber prepared in examples 1 to 4 is shown in FIG. 3. As can be seen from fig. 3, the diffraction peak of the carbon nanotube-aluminum nitride absorber prepared by the present invention includes all diffraction peaks of carbon nanotubes and aluminum nitride, and as the content of carbon nanotubes increases, the stronger the diffraction peak signal is, the higher the crystallinity is.
Example 5
Mixing the ALN @ 2% MWCNTs prepared in the embodiment 1 with paraffin according to the mass ratio of 2:3 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Measuring electromagnetic parameters (dielectric constant and magnetic permeability) of the annular carbon nanotube-aluminum nitride composite wave-absorbing material at the frequency of 2-18 GHz by using a vector network analyzer (Agilent KEYSIGHT, model number N5232B), and obtaining the wave-absorbing performance of the carbon nanotube-aluminum nitride composite wave-absorbing material by a related parameter and reflection loss calculation formula, wherein the formula is as follows:
formula (1) is a calculation formula of Reflection Loss (RL), and the unit of the reflection loss is dB;
formula (2) is input impedance (Z)in) Wherein c is the speed of light in vacuum (in m/s), f is the frequency of electromagnetic waves (in GHz), d is the thickness of the absorbing layer (in mm), and epsilonrIs a complex dielectric constant, murFor complex permeability, tanh is a hyperbolic tangent function, and j represents the complex imaginary part.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in this embodiment is shown in fig. 4, where (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 4, under the condition of the test frequency of 2-18 GHz, the wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is as follows: the real part of the dielectric constant is 5.79-5.30; the imaginary part of the dielectric constant is 1.00-1.39; the real part of the magnetic conductivity is 1.10-0.97; the imaginary part of the magnetic conductivity is 0.06 to-0.07; the lowest value of the reflection loss is-20.26 dB, the corresponding frequency appears at 17.50GHz, and the thickness of the material is 5.8 mm.
Example 6
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 with paraffin according to the mass ratio of 2:3 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in this embodiment is shown in fig. 5, where (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 5, under the condition of the test frequency of 2-18 GHz, the test wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is as follows: the real part of the dielectric constant is 12.40-5.60; the imaginary part of the dielectric constant is 6.84-3.11; the real part of the magnetic conductivity is 1.09-1.32; the imaginary part of the magnetic conductivity is 0.05 to-0.02, the lowest value of the reflection loss is-41.19 dB, the corresponding frequency is 7.41GHz, and the thickness of the material is 3.4 mm.
Example 7
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 with paraffin according to the mass ratio of 2:3 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in this embodiment is shown in fig. 6, where (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 6, under the condition of the test frequency of 2-18 GHz, the wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is as follows: the real part of the dielectric constant is 13.69-6.67; the imaginary part of the dielectric constant is 6.30-3.26; the real part of the magnetic conductivity is 0.84-1.33; the imaginary part of the magnetic permeability is 0.54 to-0.13, the lowest value of the reflection loss is-47.35 dB, the corresponding frequency is 9.08GHz, and the thickness of the material is 2.9 mm.
Example 8
Mixing the ALN @ 10% MWCNTs prepared in the embodiment 4 according to the mass ratio of 2:3 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in this embodiment is shown in fig. 7, where (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 7, under the condition of the test frequency of 2-18 GHz, the wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is as follows: the real part of the dielectric constant is 17.60-8.94; the imaginary part of the dielectric constant is 12.94-5.06; the real part of the magnetic conductivity is 1.10-1.21; the imaginary part of the magnetic conductivity is 0.05 to-0.09, the lowest value of the reflection loss is-27.38 dB, the corresponding frequency is 14.66GHz, and the thickness of the material is 1.6 mm.
Comparative example 2
Mixing the ALN @ 15% MWCNTs prepared in the comparative example 1 with paraffin according to the mass ratio of 2:3 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared by the comparative example is shown in fig. 8, wherein (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from fig. 8, the wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is measured and calculated by the method of example 5, and under the condition of the measurement frequency of 2 to 18 GHz: the real part of the dielectric constant is 8.35-4.21; the imaginary part of the dielectric constant is 2.80-3.62; the real part of the magnetic conductivity is 1.12-1.06; the imaginary part of the magnetic conductivity is 0.07 to-0.41, the lowest value of the reflection loss is-20.81 dB, the corresponding frequency is 10.64GHz, and the thickness of the material is 2.9 mm.
Example 9
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 according to the mass ratio of 3:7 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in this embodiment is shown in fig. 9, where (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 9, under the condition of the test frequency of 2-18 GHz, the wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is as follows: the real part of the dielectric constant is 9.32-4.31; the imaginary part of the dielectric constant is 3.75-4.01; the real part of the magnetic conductivity is 1.12-1.09; the imaginary part of the magnetic conductivity is 0.06 to-0.48, the lowest value of the reflection loss is-24.57 dB, the corresponding frequency is 17.36GHz, and the thickness of the material is 1.9 mm.
Example 10
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 according to the mass ratio of 3:7 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The reflection loss of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in this embodiment is shown in fig. 10, where (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 10, under the condition of the test frequency of 2-18 GHz, the wave-absorbing performance data of the carbon nanotube-aluminum nitride composite wave-absorbing material is as follows: the real part of the dielectric constant is 10.96-5.02; the imaginary part of the dielectric constant is 4.15-3.19; the real part of the magnetic permeability is 1.15-1.31; the imaginary part of the magnetic permeability is 0.08 to-0.33, the lowest value of the reflection loss is-34.42 dB, the corresponding frequency is 7.69GHz, and the thickness of the material is 3.4 mm.
Comparative example 3
Mixing the carbon nano tube with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-paraffin wave-absorbing material.
The reflection loss of the carbon nanotube-paraffin wave-absorbing material prepared by the comparative example is shown in fig. 11, wherein (a) is a reflection loss 3D diagram, and (b) is a reflection loss 2D diagram. As can be seen from FIG. 11, under the condition of the test frequency of 2-18 GHz, the wave-absorbing performance data of the carbon nanotube-paraffin wave-absorbing material is as follows: the real part of the dielectric constant is 50.64-16.35; the imaginary part of the dielectric constant is 72.28-18.11; the real part of the magnetic conductivity is 1.15-1.42; the imaginary part of the magnetic conductivity is 0.07 to-0.22, the lowest value of the reflection loss is-7.39 dB, the corresponding frequency is 15.95GHz, and the thickness of the material is 0.9 mm.
Example 11
Mixing the ALN @ 2% MWCNTs prepared in the embodiment 1 with paraffin according to the mass ratio of 1:9 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 12
Mixing the ALN @ 2% MWCNTs prepared in the embodiment 1 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 13
Mixing the ALN @ 2% MWCNTs prepared in the embodiment 1 with paraffin according to the mass ratio of 3:7 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 14
Mixing the ALN @ 2% MWCNTs prepared in the embodiment 1 with paraffin according to the mass ratio of 4:6 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The change curve of the dielectric constant and the magnetic permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 11 to 14 within the range of 2 to 18GHz is shown in fig. 12, where (a) is a real part of the dielectric constant, (b) is an imaginary part of the dielectric constant, (c) is a real part of the magnetic permeability, and (d) is an imaginary part of the magnetic permeability. As can be seen from FIG. 12, the real part of the dielectric constant is 5.79 to 5.30 in the range of the test frequency of 2 to 18 GHz; the imaginary part of the dielectric constant is 1.00-1.39; the real part of the magnetic conductivity is 1.10-0.97; the imaginary part of the magnetic conductivity is 0.06 to-0.07. The specific data of fig. 12-15 has been supplemented in the corresponding locations.
Example 15
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 with paraffin according to the mass ratio of 1:9 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 16
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 17
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 with paraffin according to the mass ratio of 3:7 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 18
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 with paraffin according to the mass ratio of 4:6 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Fig. 13 shows a change curve of the dielectric constant and the magnetic permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 15 to 18 within a range of 2 to 18GHz, where (a) is a real part of the dielectric constant, (b) is an imaginary part of the dielectric constant, (c) is a real part of the magnetic permeability, and (d) is an imaginary part of the magnetic permeability. As can be seen from FIG. 13, the real part of the dielectric constant is 12.40 to 5.60 in the range of the test frequency of 2 to 18 GHz; the imaginary part of the dielectric constant is 6.84-3.11; the real part of the magnetic conductivity is 1.09-1.32; the imaginary part of the magnetic conductivity is 0.05 to-0.02.
Example 19
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 with paraffin according to the mass ratio of 1:9 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 20
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 21
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 with paraffin according to the mass ratio of 3:7 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 22
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 with paraffin according to the mass ratio of 4:6 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
The change curve of the dielectric constant and the magnetic permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 19 to 22 within the range of 2 to 18GHz is shown in fig. 14, where (a) is a real part of the dielectric constant, (b) is an imaginary part of the dielectric constant, (c) is a real part of the magnetic permeability, and (d) is an imaginary part of the magnetic permeability. As can be seen from FIG. 14, the real part of the dielectric constant is 13.69 to 6.67 at the test frequency of 2 to 18 GHz; the imaginary part of the dielectric constant is 6.30-3.26; the real part of the magnetic conductivity is 0.84-1.33; the imaginary part of the magnetic permeability is 0.54 to-0.13.
Example 23
Mixing the ALN @ 10% MWCNTs prepared in the embodiment 4 with paraffin according to the mass ratio of 1:9 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 24
Mixing the ALN @ 10% MWCNTs prepared in the embodiment 4 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 25
Mixing the ALN @ 10% MWCNTs prepared in the embodiment 4 with paraffin according to the mass ratio of 3:7 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Example 26
Mixing the ALN @ 10% MWCNTs prepared in the embodiment 4 with paraffin according to the mass ratio of 4:6 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
Fig. 15 shows a change curve of the dielectric constant and the magnetic permeability of the carbon nanotube-aluminum nitride composite wave-absorbing material prepared in examples 23 to 26 in the range of 2 to 18GHz, where (a) is a real part of the dielectric constant, (b) is an imaginary part of the dielectric constant, (c) is a real part of the magnetic permeability, and (d) is an imaginary part of the magnetic permeability. As can be seen from FIG. 15, the real part of the dielectric constant is 17.60 to 8.94 within the range of the test frequency of 2 to 18 GHz; the imaginary part of the dielectric constant is 12.94-5.06; the real part of the magnetic conductivity is 1.10-1.21; the imaginary part of the magnetic conductivity is 0.05 to-0.09.
Example 27
Mixing the ALN @ 2% MWCNTs prepared in the embodiment 1 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
By adopting the method for testing and calculating the wave-absorbing performance data of the embodiment 5, under the condition that the test frequency is 2-18 GHz, the wave-absorbing performance data of the carbon nano tube-aluminum nitride composite wave-absorbing material is tested: the real part of the dielectric constant is 3.65-3.57; the imaginary part of the dielectric constant is 0.41-0.50; the real part of the magnetic conductivity is 1.12-0.94; the imaginary part of the magnetic conductivity is 0.06 to-0.07, the lowest value of the reflection loss is-4.93 dB, the corresponding frequency is 9.59GHz, and the thickness of the material is 4.9 mm.
Example 28
Mixing the ALN @ 5% MWCNTs prepared in the embodiment 2 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
By adopting the method for testing and calculating the wave-absorbing performance data of the embodiment 5, under the condition that the test frequency is 2-18 GHz, the wave-absorbing performance data of the carbon nano tube-aluminum nitride composite wave-absorbing material is tested: the real part of the dielectric constant is 6.54-5.26; the imaginary part of the dielectric constant is 2.14-3.37; the real part of the magnetic conductivity is 1.10-0.83; the imaginary part of the magnetic conductivity is 0.06 to-0.24, the lowest value of the reflection loss is-15.16 dB, the corresponding frequency is 17.33GHz, and the thickness of the material is 2.1 mm.
Example 29
Mixing the ALN @ 7% MWCNTs prepared in the embodiment 3 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
By adopting the method for testing and calculating the wave-absorbing performance data of the embodiment 5, under the condition that the test frequency is 2-18 GHz, the wave-absorbing performance data of the carbon nano tube-aluminum nitride composite wave-absorbing material is tested: the real part of the dielectric constant is 7.57-5.97; the imaginary part of the dielectric constant is 1.88-2.11; the real part of the magnetic conductivity is 0.83-1.00; the imaginary part of the magnetic conductivity is 0.12 to-0.08, the lowest value of the reflection loss is-21.83 dB, the corresponding frequency is 16.46GHz, and the thickness of the material is 5.7 mm.
Example 30
Mixing the ALN @ 10% MWCNTs prepared in the embodiment 4 with paraffin according to the mass ratio of 2:8 to obtain mixed powder; and (3) placing the mixed powder into an annular mold with the inner diameter of 3.04mm and the outer diameter of 7.00mm for compression molding to obtain the carbon nano tube-aluminum nitride composite wave-absorbing material.
By adopting the method for testing and calculating the wave-absorbing performance data of the embodiment 5, under the condition that the test frequency is 2-18 GHz, the wave-absorbing performance data of the carbon nano tube-aluminum nitride composite wave-absorbing material is tested: the real part of the dielectric constant is 8.35-4.21; the imaginary part of the dielectric constant is 2.80-3.62; the real part of the magnetic conductivity is 1.12-1.06; the imaginary part of the magnetic conductivity is 0.07 to-0.41, the lowest value of the reflection loss is-20.91 dB, the corresponding frequency is 10.64GHz, and the thickness of the material is 2.9 mm.
In conclusion, the carbon nanotube-aluminum nitride composite wave-absorbing material prepared by the invention has excellent wave-absorbing performance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A carbon nanotube-aluminum nitride wave absorber is characterized by comprising a carbon nanotube and aluminum nitride; the aluminum nitride is coated on the surface of the carbon nano tube;
the mass of the carbon nano tube accounts for 1-10% of the total mass of the carbon nano tube-aluminum nitride wave absorber.
2. The carbon nanotube-aluminum nitride absorber according to claim 1, wherein the carbon nanotube has an outer diameter of 30 to 50 nm; the length of the carbon nanotube is 2-10 mu m.
3. The carbon nanotube-aluminum nitride absorber according to claim 1, wherein the aluminum nitride is needle-shaped, has a length of 60 to 120nm, and has a diameter of 5 to 15 nm.
4. The method for preparing the carbon nanotube-aluminum nitride absorber according to any one of claims 1 to 3, comprising the steps of:
mixing the carbon nano tube, the aluminum nitride and the anhydrous dispersant, and carrying out modification treatment to obtain the carbon nano tube-aluminum nitride wave absorber.
5. The method of claim 4, wherein the mixing is ultrasonic dispersion; the ultrasonic dispersion time is 60-180 min.
6. The preparation method according to claim 4, wherein the temperature of the modification treatment is 80 to 160 ℃, the time is 4 to 10 hours, and the rate of heating to the modification treatment temperature is 2 to 4 ℃/min.
7. The carbon nanotube-aluminum nitride absorber according to claim 4, wherein the anhydrous dispersant comprises anhydrous N, N-dimethylformamide or anhydrous ethanol.
8. A carbon nanotube-aluminum nitride composite wave-absorbing material is characterized by comprising a carbon nanotube-aluminum nitride wave-absorbing agent and paraffin;
the carbon nanotube-aluminum nitride wave absorber is the carbon nanotube-aluminum nitride wave absorber according to any one of claims 1 to 3 or the carbon nanotube-aluminum nitride wave absorber prepared by the preparation method according to any one of claims 4 to 7.
9. The carbon nanotube-aluminum nitride composite wave-absorbing material according to claim 8, wherein the mass ratio of the carbon nanotube-aluminum nitride wave-absorbing agent to the paraffin is 1: 9-2: 3.
10. The carbon nanotube-aluminum nitride composite wave-absorbing material of any one of claims 8 to 9, which is applied to a thermosensitive element, a photosensitive element, an electronic element, an intelligent element or a sensor.
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