CN111978742A - Preparation method of carbon fiber wave-absorbing material with dielectric and eddy current losses - Google Patents
Preparation method of carbon fiber wave-absorbing material with dielectric and eddy current losses Download PDFInfo
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Abstract
The invention relates to the technical field of wave-absorbing materials, in particular to a preparation method of a carbon fiber wave-absorbing material with dielectric and eddy current losses. The invention solves the problems that the carbon fundamental wave material in the prior art only has dielectric loss and poor magnetic loss, and the prepared carbon fiber wave-absorbing material not only has dielectric loss characteristics, but also has eddy current loss characteristics because the carbon fibers which are mutually bridged cause skin effect in the structural aspect, thereby being superior to the traditional carbon-based wave-absorbing material and being applicable to the fields of aircraft stealth coatings and the like.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a preparation method of a carbon fiber wave-absorbing material with dielectric loss and eddy current loss characteristics.
Background
Wave-absorbing materials are a class of materials that can absorb or substantially attenuate the energy of electromagnetic waves received at their surfaces, thereby reducing the interference of electromagnetic waves. In engineering application, the wave-absorbing material is required to have high absorption rate to electromagnetic waves in a wider frequency band, and also required to have the properties of light weight, temperature resistance, moisture resistance, corrosion resistance and the like. With the development of modern science and technology, whether military or civil electromagnetic waves are closely related to human beings, the influence of electromagnetic wave radiation on the environment is increasingly increased. The airplane and airplane flight are mistakenly started because the airplane and airplane flight cannot take off due to electromagnetic wave interference; in hospitals and mobile phones, the normal operation of various electronic medical instruments is often interfered. Therefore, the material which can resist and weaken electromagnetic wave radiation is searched for after the electromagnetic pollution is treated, the wave-absorbing material is greatly concerned as a medium which can effectively shield electromagnetic waves, and the material has great application value particularly in the relevant fields of military radar stealth coatings and the like.
Carbon materials have the advantages of high dielectric constant, low density, structural diversity, etc., and are favored by researchers. The carbon-based wave-absorbing material is widely applied to skin materials at positions of flaps, aileron rudders and the like of stealth fighters such as Mige-29, phantom 2000, gust and the like.
The loss mechanism of the common carbon-based wave-absorbing material at present is dielectric loss, such as graphite, carbon black and the like, but the magnetic loss capacity of the carbon-based wave-absorbing material is very weak, so that the carbon-based wave-absorbing material is often used as a matrix material to be compounded with magnetic materials such as ferroferric oxide and the like, and the preparation process of the composite material is relatively complicated, so that the prepared composite wave-absorbing material has great difficulty in practical use.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a carbon fiber wave-absorbing material with dielectric loss and eddy current loss characteristics, wherein a fibrous product obtained by performing electrostatic spinning on a water solution of polyvinyl alcohol and diammonium hydrogen phosphate is used as a precursor, and the precursor is subjected to preoxidation in air and high-temperature carbonization in inert gas, is uniformly mixed and dispersed with paraffin in acetone, and is then cured and molded.
The specific technical scheme is as follows:
a preparation method of a carbon fiber wave-absorbing material with dielectric and eddy current losses is characterized in that a fibrous product obtained by performing electrostatic spinning on a water solution of polyvinyl alcohol and diammonium hydrogen phosphate is used as a precursor, the precursor is subjected to preoxidation in air and high-temperature carbonization in inert gas, and the carbon fiber wave-absorbing material is finally prepared, and the preparation method comprises the following specific steps:
(1) preparing a mixed aqueous solution of polyvinyl alcohol and diammonium hydrogen phosphate: mixing polyvinyl alcohol and diammonium hydrogen phosphate with deionized water, uniformly stirring for 3-5 hours at 90-95 ℃, and cooling to room temperature to obtain a mixed aqueous solution of 5-15% of polyvinyl alcohol and 1-5% of diammonium hydrogen phosphate in mass fraction;
(2) preparing a precursor: adding the mixed aqueous solution into an injector, wherein the injector uses an industrial flat-head needle, and electrostatic spinning is carried out on a cylindrical collector rotating at the speed of 50-200 rpm by using electrostatic spinning equipment under the condition of applying 10-25 kV voltage and the feeding speed of 100-800 mu L/h, the distance between the collector and a needle point is 8-20 cm, and finally, a white fabric of the nanofiber containing diammonium phosphate in polyvinyl alcohol is obtained as a precursor;
(3) preoxidation and high-temperature carbonization of the precursor: putting the precursor into a ceramic crucible without a cover, placing the ceramic crucible into a tubular furnace for pre-oxidation at the temperature of 200-300 ℃, the pre-oxidation time of 20-120 min, the temperature rise rate of 5 ℃/min, carrying out the whole pre-oxidation process in the air, inducing intramolecular dehydration of polyvinyl alcohol through diammonium hydrogen phosphate, carrying out high-temperature carbonization after the pre-oxidation process is finished, wherein the carbonization temperature is 600-1000 ℃, the carbonization time is 20-60 min, the temperature rise rate is 5 ℃/min, continuously introducing inert gas in the whole carbonization process to isolate oxygen, and cooling to room temperature to obtain carbon fibers;
(4) curing and forming: fully mixing the carbon fibers with paraffin according to the mass ratio of 1 (0.5-2), adding a certain amount of acetone, uniformly dispersing by ultrasonic oscillation, evaporating the acetone in a water bath at 60 ℃, drying the residual mixture, and naturally cooling to obtain the carbon fiber wave-absorbing material.
The viscosity of the polyvinyl alcohol in the step (1) is 40.0-48.0 Pa.s, and the alcoholysis degree is 87.0-89.0 mol%.
The mass ratio of the acetone to the carbon fibers in the step (4) is 8: 1.
compared with the prior art, the invention has the following beneficial technical effects:
1. the raw material industrial preparation technology is mature, the price is low, the material belongs to an environment-friendly material, no harmful substance is generated in the preparation process, and the stability and the repeatability are good.
2. The carbon fiber wave-absorbing material prepared by the invention has excellent absorption performance in C wave band, X wave band and Ku wave band, strong absorption capacity, wide range of effective absorption bandwidth, low minimum thickness for satisfying effective loss (-10dB), and light and thin, and the preparation process is selected according to the actual application requirements.
3. The carbon fiber wave-absorbing material prepared by the invention not only has dielectric loss characteristic, but also has eddy current loss characteristic because the carbon fibers which are mutually bridged cause skin effect in the aspect of structure, is superior to the traditional carbon-based wave-absorbing material, and can be applied to the fields of aircraft stealth coatings and the like.
Drawings
FIG. 1 is a reflection loss spectrum of a carbon fiber wave-absorbing material subjected to carbonization at 600 ℃ for 20min in example 1;
FIG. 2 is a reflection loss spectrum of the carbon fiber wave-absorbing material in example 1, which is carbonized at 600 ℃ for 20min and corresponds to different thicknesses;
FIG. 3 is a real part and imaginary part spectrum of the magnetic permeability of the carbon fiber wave-absorbing material after carbonization at 600 ℃ for 20min in example 1.
FIG. 4 is a reflection loss spectrum of the carbon fiber wave-absorbing material after carbonization at 1000 ℃ for 60min in example 2;
FIG. 5 is a reflection loss spectrum of the carbon fiber wave-absorbing material in example 2, which is carbonized at 1000 ℃ for 60min and corresponds to different thicknesses;
FIG. 6 is a real part and imaginary part spectrum of the magnetic permeability of the carbon fiber wave-absorbing material after carbonization at 1000 ℃ for 60min in example 2.
FIG. 7 is a reflection loss spectrum of the carbon fiber wave-absorbing material obtained in example 3 after carbonization at 850 ℃ for 30 min;
FIG. 8 is a reflection loss spectrum of the carbon fiber wave-absorbing material in example 3, which is carbonized at 850 ℃ for 30min and corresponds to different thicknesses;
FIG. 9 is a real part and imaginary part spectrum of the magnetic permeability of the carbon fiber wave-absorbing material after carbonization at 850 ℃ for 30min in example 3.
Detailed Description
The present invention is described in detail below with reference to the drawings and examples, but the scope of the present invention is not limited by the drawings and examples.
Example 1:
a preparation method of a carbon fiber wave-absorbing material with dielectric loss and eddy current loss characteristics comprises the following specific steps:
(1) preparing a mixed aqueous solution of polyvinyl alcohol and diammonium hydrogen phosphate: mixing polyvinyl alcohol and diammonium hydrogen phosphate with deionized water, uniformly stirring for 3 hours at 90 ℃, and cooling to room temperature to obtain a mixed aqueous solution of 5 mass percent of polyvinyl alcohol and 1 mass percent of diammonium hydrogen phosphate; the viscosity of the polyvinyl alcohol is 40.0Pa.s, and the alcoholysis degree is 87.0 mol%.
(2) Preparing a precursor: adding the mixed aqueous solution into an injector, wherein the injector uses an industrial flat-head needle, and electrostatic spinning is carried out on a cylindrical collector rotating at the speed of 50rpm by using electrostatic spinning equipment under the conditions of applying 10kV voltage and feeding speed of 100 mu L/h, the distance between the collector and a needle point is 8cm, and finally, a white fabric of the nanofiber containing diammonium phosphate in the polyvinyl alcohol is obtained as a precursor;
(3) preoxidation and high-temperature carbonization of the precursor: putting the precursor into a ceramic crucible without a cover, placing the ceramic crucible into a tubular furnace for pre-oxidation at the temperature of 200 ℃, the pre-oxidation time of 20min, the temperature rise rate of 5 ℃/min, carrying out the whole pre-oxidation process in the air, inducing the intramolecular dehydration of polyvinyl alcohol through diammonium hydrogen phosphate, carrying out high-temperature carbonization after the pre-oxidation process is finished, wherein the carbonization temperature is 600 ℃, the carbonization time is 20min, the temperature rise rate is 5 ℃/min, continuously introducing inert gas in the whole carbonization process to isolate oxygen, and cooling to room temperature to obtain carbon fibers; .
(4) Curing and forming: fully mixing the carbon fibers with paraffin according to a mass ratio of 1:0.5, adding a certain amount of acetone, wherein the mass ratio of the acetone to the carbon fibers is 8: 1, uniformly dispersing by ultrasonic oscillation, evaporating acetone in a water bath at 60 ℃, drying the residual mixture, and naturally cooling to obtain the carbon fiber wave-absorbing material.
Fig. 1 is a reflection loss spectrum of a carbon fiber wave-absorbing material after being carbonized at 600 ℃ for 20min in example 1, fig. 2 is a reflection loss spectrum of the carbon fiber wave-absorbing material after being carbonized at 600 ℃ for 20min in example 1, the reflection loss spectra correspond to different thicknesses, and fig. 3 is a real part and an imaginary part spectrum of the magnetic permeability of the carbon fiber wave-absorbing material after being carbonized at 600 ℃ for 20min in example 1, as shown in fig. 1 and 2: the optimal reflection loss thickness of the carbon fiber wave-absorbing material is 2.76mm, the lowest reflection loss is-44.98 dB, the peak value is 10.86GHz, the effective bandwidth smaller than-10 dB is 3.8GHz, and the X wave band is 8-12 GHz, so that the carbon fiber wave-absorbing material has excellent wave-absorbing performance in the X wave band, absorbs most strongly under 10.86GHz, can reach more than 99.9 percent, and can absorb 3.8GHz effectively. And also shows good wave absorbing performance in C and Ku wave bands. As shown in fig. 3, the imaginary part of the magnetic permeability of the carbon fiber wave-absorbing material is greater than 0, and it can be seen that the carbon fiber wave-absorbing material has not only dielectric loss but also eddy current loss.
Example 2:
a preparation method of a carbon fiber wave-absorbing material with dielectric loss and eddy current loss characteristics comprises the following specific steps:
(1) preparing a mixed aqueous solution of polyvinyl alcohol and diammonium hydrogen phosphate: mixing polyvinyl alcohol and diammonium hydrogen phosphate with deionized water, uniformly stirring for 5 hours at 95 ℃, and cooling to room temperature to obtain a mixed aqueous solution of 15 mass percent of polyvinyl alcohol and 5 mass percent of diammonium hydrogen phosphate; the viscosity of the polyvinyl alcohol is 48.0Pa.s, and the alcoholysis degree is 89.0 mol%.
(2) Preparing a precursor: adding the mixed aqueous solution into an injector, wherein the injector uses an industrial flat-head needle, and electrostatic spinning is carried out on a cylindrical collector rotating at the speed of 200rpm by using electrostatic spinning equipment under the conditions of applying 25kV voltage and the feeding speed of 800 mu L/h, the distance between the collector and a needle point is 20cm, and finally, a white fabric containing the nanofibers of diammonium phosphate in polyvinyl alcohol is obtained as a precursor;
(3) preoxidation and high-temperature carbonization of the precursor: putting the precursor into a ceramic crucible without a cover, placing the ceramic crucible into a tubular furnace for pre-oxidation at the temperature of 300 ℃, the pre-oxidation time of 120min and the heating rate of 5 ℃/min, carrying out the whole pre-oxidation process in the air, inducing the intramolecular dehydration of polyvinyl alcohol through diammonium hydrogen phosphate, carrying out high-temperature carbonization after the pre-oxidation process is finished, wherein the carbonization temperature is 1000 ℃, the carbonization time is 60min and the heating rate is 5 ℃/min, continuously introducing inert gas in the whole carbonization process to isolate oxygen, and cooling to room temperature to obtain carbon fibers;
(4) curing and forming: fully mixing the carbon fibers with paraffin according to a mass ratio of 1:2, adding a certain amount of acetone, wherein the mass ratio of the acetone to the carbon fibers is 8: 1, uniformly dispersing by ultrasonic oscillation, evaporating acetone in a water bath at 60 ℃, drying the residual mixture, and naturally cooling to obtain the carbon fiber wave-absorbing material.
Fig. 4 is a reflection loss spectrum of the carbon fiber wave-absorbing material after carbonization at 1000 ℃ for 60min in example 2, fig. 5 is a reflection loss spectrum of the carbon fiber wave-absorbing material after carbonization at 1000 ℃ for 60min in example 2, which corresponds to different thicknesses, and fig. 6 is a real part and an imaginary part spectrum of the magnetic permeability of the carbon fiber wave-absorbing material after carbonization at 1000 ℃ for 60min in example 2, as shown in fig. 4 and 5: the optimal reflection loss thickness of the carbon fiber wave-absorbing material is 1.09mm, the lowest reflection loss is-46.18 dB, the peak value is corresponding to 16.13GHz, the effective bandwidth smaller than-10 dB is 3GHz, the second optimal reflection loss thickness is 2.50mm, the lowest reflection loss is-42.66 dB, the peak value is corresponding to 7.97GHz, the effective bandwidth smaller than-10 dB is 2GHz, the C wave band is 4-8 GHz, and the Ku wave band is 12-18 GHz, so that the carbon fiber wave-absorbing material has excellent wave-absorbing performance in C and Ku wave bands, is most strongly absorbed at 16.13GHz, can reach more than 99.9%, and can absorb the effective bandwidth of 3 GHz. And also shows good wave absorbing performance in the X section. As shown in fig. 6, the imaginary part of the magnetic permeability of the carbon fiber wave-absorbing material is greater than 0, and it can be seen that the carbon fiber wave-absorbing material has not only dielectric loss but also eddy current loss.
Example 3:
a preparation method of a carbon fiber wave-absorbing material with dielectric loss and eddy current loss characteristics comprises the following specific steps:
(1) preparing a mixed aqueous solution of polyvinyl alcohol and diammonium hydrogen phosphate: mixing polyvinyl alcohol and diammonium hydrogen phosphate with deionized water, uniformly stirring for 4 hours at 93 ℃, and cooling to room temperature to obtain a mixed aqueous solution of 10 mass percent of polyvinyl alcohol and 3 mass percent of diammonium hydrogen phosphate; the viscosity of the polyvinyl alcohol is 45.0Pa.s, and the alcoholysis degree is 88.0 mol%.
(2) Preparing a precursor: adding the mixed aqueous solution into an injector, wherein the injector uses an industrial flat-head needle, and electrostatic spinning is carried out on a cylindrical collector rotating at the speed of 100rpm by using electrostatic spinning equipment under the conditions of applying 15kV voltage and feeding speed of 500 mu L/h, the distance between the collector and a needle point is 10cm, and finally, a white fabric of the nanofiber containing diammonium phosphate in the polyvinyl alcohol is obtained as a precursor;
(3) preoxidation and high-temperature carbonization of the precursor: putting the precursor into a ceramic crucible without a cover, placing the ceramic crucible into a tubular furnace for pre-oxidation at the temperature of 250 ℃, the pre-oxidation time of 30min and the heating rate of 5 ℃/min, carrying out the whole pre-oxidation process in the air, inducing the intramolecular dehydration of polyvinyl alcohol through diammonium hydrogen phosphate, carrying out high-temperature carbonization after the pre-oxidation process is finished, wherein the carbonization temperature is 850 ℃, the carbonization time is 30min and the heating rate is 5 ℃/min, continuously introducing inert gas in the whole carbonization process to isolate oxygen, and cooling to room temperature to obtain carbon fibers;
(4) curing and forming: fully mixing the carbon fibers and paraffin according to a mass ratio of 1:1, adding a certain amount of acetone, uniformly dispersing by ultrasonic oscillation, evaporating the acetone in a water bath at 60 ℃, drying the residual mixture, and naturally cooling to obtain the carbon fiber wave-absorbing material; the mass ratio of the acetone to the carbon fibers is 8: 1.
fig. 7 is a reflection loss spectrum of the carbon fiber wave-absorbing material after being carbonized at 850 ℃ for 30min in example 3, fig. 8 is a reflection loss spectrum of the carbon fiber wave-absorbing material after being carbonized at 850 ℃ for 30min in example 3, which corresponds to different thicknesses, and fig. 9 is a real part and an imaginary part spectrum of the magnetic permeability of the carbon fiber wave-absorbing material after being carbonized at 850 ℃ for 30min in example 3, as shown in fig. 7 and 8: the optimal reflection loss thickness of the carbon fiber wave-absorbing material is 1.17mm, the lowest reflection loss is-44.40 dB, the peak value is corresponding to 14.94GHz, the effective bandwidth smaller than-10 dB is 3.6GHz, the second optimal reflection loss thickness is 2.50mm, the lowest reflection loss is-43.35 dB, the peak value is corresponding to 7.46GHz, the effective bandwidth smaller than-10 dB is 1.9GHz, the C wave band is 4-8 GHz, and the Ku wave band is 12-18 GHz, so that the carbon fiber wave-absorbing material has excellent wave-absorbing performance in C and Ku wave bands, can absorb most strongly at 14.94GHz, can reach more than 99.9%, and can absorb the effective bandwidth of 3.6 GHz. And also shows good wave absorbing performance in the X section. As shown in fig. 9, the imaginary part of the magnetic permeability of the carbon fiber wave-absorbing material is greater than 0, and it can be seen that the carbon fiber wave-absorbing material has not only dielectric loss but also eddy current loss.
Claims (3)
1. A preparation method of a carbon fiber wave-absorbing material with dielectric and eddy current losses is characterized in that a fibrous product obtained by electrostatic spinning of a water solution of polyvinyl alcohol and diammonium hydrogen phosphate is used as a precursor, the precursor is subjected to preoxidation in air and high-temperature carbonization in inert gas, and the carbon fiber wave-absorbing material is finally prepared, and the specific steps are as follows:
(1) preparing a mixed aqueous solution of polyvinyl alcohol and diammonium hydrogen phosphate: mixing polyvinyl alcohol and diammonium hydrogen phosphate with deionized water, uniformly stirring for 3-5 hours at 90-95 ℃, and cooling to room temperature to obtain a mixed aqueous solution of 5-15% of polyvinyl alcohol and 1-5% of diammonium hydrogen phosphate in mass fraction;
(2) preparing a precursor: adding the mixed aqueous solution into an injector, wherein the injector uses an industrial flat-head needle, and electrostatic spinning is carried out on a cylindrical collector rotating at the speed of 50-200 rpm by using electrostatic spinning equipment under the condition of applying 10-25 kV voltage and the feeding speed of 100-800 mu L/h, the distance between the collector and a needle point is 8-20 cm, and finally, a white fabric of the nanofiber containing diammonium phosphate in polyvinyl alcohol is obtained as a precursor;
(3) preoxidation and high-temperature carbonization of the precursor: putting the precursor into a ceramic crucible without a cover, placing the ceramic crucible into a tubular furnace for pre-oxidation at the temperature of 200-300 ℃, the pre-oxidation time of 20-120 min, the temperature rise rate of 5 ℃/min, carrying out the whole pre-oxidation process in the air, inducing intramolecular dehydration of polyvinyl alcohol through diammonium hydrogen phosphate, carrying out high-temperature carbonization after the pre-oxidation process is finished, wherein the carbonization temperature is 600-1000 ℃, the carbonization time is 20-60 min, the temperature rise rate is 5 ℃/min, continuously introducing inert gas in the whole carbonization process to isolate oxygen, and cooling to room temperature to obtain carbon fibers;
(4) curing and forming: fully mixing the carbon fibers with paraffin according to the mass ratio of 1 (0.5-2), adding a certain amount of acetone, uniformly dispersing by ultrasonic oscillation, evaporating the acetone in a water bath at 60 ℃, drying the residual mixture, and naturally cooling to obtain the carbon fiber wave-absorbing material.
2. The preparation method of the carbon fiber wave-absorbing material with dielectric and eddy current loss according to claim 1, characterized in that: the viscosity of the polyvinyl alcohol in the step (1) is 40.0-48.0 Pa.s, and the alcoholysis degree is 87.0-89.0 mol%.
3. The preparation method of the carbon fiber wave-absorbing material with dielectric and eddy current loss according to claim 1, characterized in that: the mass ratio of the acetone to the carbon fibers in the step (4) is 8: 1.
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| RU2782268C1 (en) * | 2022-02-21 | 2022-10-25 | Общество с ограниченной ответственностью "Научно-производственная компания "Энергия" | Method for manufacturing electrically conductive material |
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| US4728395A (en) * | 1984-10-12 | 1988-03-01 | Stackpole Fibers Company, Inc. | Controlled resistivity carbon fiber paper and fabric sheet products and method of manufacture |
| CA2417247A1 (en) * | 2000-07-26 | 2002-01-31 | Ballard Power Systems Inc. | Carbon-matrix composites, compositions and methods related thereto |
| CN102382623A (en) * | 2011-08-02 | 2012-03-21 | 山东大学 | Preparation method of carbon-based composite wave-absorbing material |
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| RU2782268C1 (en) * | 2022-02-21 | 2022-10-25 | Общество с ограниченной ответственностью "Научно-производственная компания "Энергия" | Method for manufacturing electrically conductive material |
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