CN113652769B - Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption - Google Patents
Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption Download PDFInfo
- Publication number
- CN113652769B CN113652769B CN202111003104.4A CN202111003104A CN113652769B CN 113652769 B CN113652769 B CN 113652769B CN 202111003104 A CN202111003104 A CN 202111003104A CN 113652769 B CN113652769 B CN 113652769B
- Authority
- CN
- China
- Prior art keywords
- coaxial
- core
- shell
- fiber
- wave absorber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Inorganic Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a core-shell Fe 3 The preparation of the C/C fiber composite wave absorber and the application thereof in microwave absorption comprise: dissolving polyacrylonitrile and ferric nitrate in an organic solvent, mixing and stirring until the mixture is clear to obtain a mixed solution; coaxially spinning a stainless steel needle head, and putting the mixed solution into a needle cylinder to be used as an external phase; taking ferric nitrate solution as an internal phase; the flow speed is regulated by a micro-injection pump, a direct current power supply is connected to a coaxial spinning stainless steel needle, and coaxial fibers are manufactured by a coaxial electrostatic spinning method; placing the collected coaxial fibers into a muffle furnace, and performing pre-oxidation in air to obtain pre-oxidized fibers; the pre-oxidized fiber is put into a tube furnace and carbonized and sintered into core-shell Fe in Ar atmosphere 3 C/C doped carbon fiber, fe provided by the invention 3 The C-doped carbon fiber is obtained by integrally forming through an electrostatic spinning technology, and has the advantages of high manufacturing efficiency, low environmental requirement and simple post-treatment; and can obtain better broadband wave absorbing performance under lower iron content.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to preparation of a core-shell Fe3C/C fiber composite wave-absorbing agent and application thereof in microwave absorption.
Background
The rapid development of electromagnetic technology has increasingly stringent requirements for electromagnetic wave absorbing materials. In the military field, the aircraft and the submersible are required to realize stealth of radar waves, and various electromagnetic signals with important information are also required to be protected so as to prevent leakage and theft; in the field of civilian life, the wide application of electronic and electrical equipment is accompanied by increasingly serious electromagnetic radiation problems, and the health and natural environment of a human body are seriously affected. Therefore, it is of great importance to develop electromagnetic wave absorbing materials having high performance.
At present, no perfect wave absorbing material has ideal performance requirements of thin thickness, wide absorption frequency band, low reflection loss and light weight. The traditional wave absorbing material mainly comprises metal micro powder, ferrite and carbon material, and electromagnetic wave absorption is realized through magnetic loss and dielectric loss, but the wave absorbing bandwidth, environmental resistance, density and the like of the traditional wave absorbing material still have related problems due to the intrinsic property of the material. Thanks to the progress of nano technology, the size, shape, structure and composition of the material can be regulated and controlled in a larger range, thereby promoting the development of the wave-absorbing material towards composite materials, multiband compatibility, intellectualization and the like.
The carbon material has the advantages of light weight, excellent conductivity, good stability, low price and the like, but cannot meet the application requirements of the wave-absorbing material due to lower electromagnetic loss intensity. It can be seen that once the problem of its single loss is overcome, carbon materials will become one of the important future for wave absorbing materials. Many researchers compound carbon materials with other electrically or magnetically lossy wave absorbing materials, thereby introducing more absorption mechanisms, improving impedance matching characteristics and obtaining better results. However, most of the carbon wave absorber materials reported at present are gel particles or films, the preparation process is long, the process is complex, and large-scale application is difficult to obtain.
In view of the situation, the core-shell type composite carbon fiber loaded with ferromagnetic particles is prepared by adopting a coaxial electrostatic spinning technology, the magnetic particles are uniformly embedded into the fiber by blending a magnetic particle solution and a polyacrylonitrile solution, and then the fiber is subjected to high-temperature treatment to obtain the Fe3C/C fiber composite wave absorber with different morphologies, so that broadband absorption can be realized.
Disclosure of Invention
The invention aims to provide a magnetic particle doped core-shell carbon fiber and an integrated manufacturing method thereof. The carbon fiber has dielectric loss and magnetic loss, has strong absorption to radar waves, and can be used as a wave absorber.
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a core-shell type Fe 3 The preparation method of the C/C fiber composite wave absorber comprises the following steps:
step one, dissolving polyacrylonitrile and ferric nitrate in an organic solvent, mixing and stirring until the mixture is clear to obtain a mixed solution;
step two, adopting a coaxial spinning stainless steel needle head, and putting the mixed liquid in the step one into a needle cylinder to be used as an external phase; taking ferric nitrate solution as an internal phase; the flow speed is regulated by a micro-injection pump, a direct current power supply is connected to a coaxial spinning stainless steel needle, and coaxial fibers are manufactured by a coaxial electrostatic spinning method;
step three, placing the coaxial fibers collected in the step two into a muffle furnace, and pre-oxidizing in air to obtain pre-oxidized fibers;
step four, placing the pre-oxidized fiber into a tubular furnace, and carbonizing and sintering the pre-oxidized fiber into core-shell Fe in Ar atmosphere 3 C/C doped carbon fiber, i.e. core-shell Fe 3 C/C fiber composite wave absorber.
Preferably, in the first step, the organic solvent is N, N-dimethylformamide and/or N-methylpyrrolidone.
Preferably, in the first step, the molecular weight of the polyacrylonitrile is 5 ten thousand to 15 ten thousand, and the concentration of the polyacrylonitrile in the mixed solution is 3wt percent to 15wt percent.
Preferably, in the first step, the concentration of the ferric nitrate in the mixed solution is 0wt percent to 5wt percent; in the second step, the concentration of the ferric nitrate solution is 1-5 wt%.
Preferably, in the second step, the coaxial electrostatic spinning method includes the following technological parameters: the flow rate of the external phase microinjection pump is 0.4-1 mL/h, the flow rate of the internal phase microinjection pump is 0.2-0.5 mL/h, and the flow rate ratio of the internal phase to the external phase is 1:2; the voltage of the direct current power supply is 5 kV-15 kV, and the distance between the coaxial spinning stainless steel needle head and the fiber receiving substrate is 8-12 cm; the coaxial electrostatic spinning is carried out in a constant temperature and humidity box, the temperature is controlled to be 15-25 ℃, and the humidity is controlled to be 40-60%.
Preferably, in the third step, the pre-oxidation temperature is 280-320 ℃, the heating rate is 1.5-3 ℃/min, and the heat preservation time is 1.5-2.5 h.
Preferably, in the fourth step, the carbonization temperature is 800-1200 ℃, the heating rate is 4-7 ℃/min, and the heat preservation time is 1.5-2.5 h.
Preferably, in the first step, the polyacrylonitrile is pretreated before use, and the pretreatment process is as follows: treating polyacrylonitrile powder by adopting low-temperature plasma; the low-temperature plasma is dielectric barrier discharge plasma; the conditions for processing the polyacrylonitrile powder by the low-temperature plasma are as follows: in CF 4 Or CCl 4 In the atmosphere, the current is 1.5-2.5A, the voltage is 90-110V, and the discharge time is 1.5-3.5 min.
Preferably, in the fourth step, the carbonization process is as follows: heating to 300-450 ℃ at a heating rate of 2.5 ℃/min, preserving heat for 30-60 min, then heating to 600-800 ℃ at a heating rate of 5 ℃/min, preserving heat for 30-60 min, then heating to 1000-1200 ℃ at a heating rate of 5 ℃/min, and preserving heat for 90-120 min.
The invention also provides a core-shell Fe as described above 3 The application of the C/C fiber composite wave absorber in microwave absorption.
The invention at least comprises the following beneficial effects:
compared with the prior art, the Fe provided by the invention 3 The C-doped carbon fiber is obtained by integrally forming through an electrostatic spinning technology, and has the advantages of high manufacturing efficiency, low environmental requirement and simple post-treatment; and can obtain better broadband wave-absorbing performance under lower iron content; prepared core-shell Fe 3 The C/C fiber composite wave absorber obtains a reflection loss peak value smaller than-10 dB at 2-18 GHz;
the fiber wave absorber provided by the invention has a controllable microstructure, the integrated formation of the magnetic particles and the carbon fibers can reduce the aggregation of the magnetic particles from the molecular level, improve the uniformity of doped fibers, increase the interface loss due to a core-shell structure, and simultaneously realize the control of the wave absorbing performance of the fiber wave absorber through the microstructure regulation because the carbon fibers have rich pore structures due to the activation of Fe. When electromagnetic waves enter the core-shell carbon fiber, reflection, scattering and other processes can occur; and the reflected and scattered electromagnetic wave can generate new reflection and scattering again after encountering the fiber wall. The repeated reflection and scattering can attenuate electromagnetic waves and dissipate the electromagnetic waves through heat energy, so that the microwave absorption performance of the carbon fiber subjected to high-temperature heat treatment is greatly improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 shows a core-shell Fe prepared according to an embodiment of the present invention 3 Electromagnetic parameters of the C/C fiber composite wave absorber;
FIG. 2 shows a core-shell Fe prepared according to an embodiment of the present invention 3 Reflection loss of the C/C fiber composite wave absorber;
FIG. 3 shows a core-shell Fe prepared according to an embodiment of the present invention 3 The wave absorption bandwidth of the C/C fiber composite wave absorber;
FIG. 4 shows a core-shell Fe prepared in example 1 of the present invention 3 TEM photographs of C/C fiber composite wave absorbers.
The specific embodiment is as follows:
the present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
core-shell type Fe 3 The preparation method of the C/C fiber composite wave absorber comprises the following steps:
step one, dissolving polyacrylonitrile and ferric nitrate in N, N-dimethylformamide, mixing and stirring until the mixture is clear, and obtaining a mixed solution; the concentration of polyacrylonitrile in the mixed solution is 10wt%; the concentration of ferric nitrate in the mixed solution is 3wt%;
step two, adopting a coaxial spinning stainless steel needle head, and putting the mixed liquid in the step one into a needle cylinder to be used as an external phase; simultaneously taking an iron nitrate solution with the concentration of 5 weight percent as an internal phase; the flow speed is regulated by a micro-injection pump, a direct current power supply is connected to a coaxial spinning stainless steel needle, and coaxial fibers are manufactured by a coaxial electrostatic spinning method; the coaxial electrostatic spinning method comprises the following technological parameters: the flow rate of the external phase microinjection pump is 0.8mL/h, the flow rate of the internal phase microinjection pump is 0.4mL/h, and the flow rate ratio of the internal phase to the external phase is 1:2; the voltage of the direct current power supply is 8kV, and the distance between the coaxial spinning stainless steel needle head and the fiber receiving substrate is 10cm; the coaxial electrostatic spinning is carried out in a constant temperature and humidity box, the temperature is controlled at 20 ℃, and the humidity is controlled at 50%;
step three, the coaxial fibers collected in the step two are put into a muffle furnace, and pre-oxidized in air to obtain pre-oxidized fibers; the pre-oxidation temperature is 300 ℃, the heating rate is 2.5 ℃/min, and the heat preservation time is 2 hours;
step four, placing the pre-oxidized fiber into a tubular furnace, and carbonizing and sintering the pre-oxidized fiber into core-shell Fe in Ar atmosphere 3 C/C doped carbon fiber, i.e. core-shell Fe 3 C/C fiber composite wave absorber; the carbonization temperature of the fiber is 800 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 2 hours; core-shell Fe prepared in this example 3 The C/C fiber composite wave absorber has the maximum reflection loss when the thickness is 2.50mmThe consumption value was-20.6 dB.
FIG. 1 shows core-shell Fe prepared in example 1 3 A graph of electromagnetic parameters of the C/C fiber composite wave absorber along with frequency change; the vector network analyzer is used for testing core-shell Fe 3 Electromagnetic parameters and electromagnetic wave absorption performance of the C/C fiber composite wave absorber; the instrument model was PNA N5244A vector network analyzer from agilent, usa; the sample adopts a coaxial mode test, firstly core-shell Fe 3 Grinding the C/C fibers into powder, mixing with paraffin wax at a ratio of 10wt%, pressing into an annular sample with an inner diameter of 3.04mm, an outer diameter of 7.00mm and a thickness of 2.00mm in a coaxial ring die, testing the frequency of 2-18GHz, testing the dielectric constant and the magnetic conductivity, and calculating the electromagnetic wave absorption performance of the material by utilizing a transmission line theory;
as can be seen from FIG. 1, core-shell Fe in the entire band of 2-18GHz 3 The values of the real part epsilon 'and the imaginary part epsilon' of the dielectric constant of the C/C fiber composite wave absorber are reduced along with the increase of the frequency. The cause of the decrease in dielectric constant is space charge polarization and orientation polarization due to charge confinement. The frequency dispersion behavior is commonly found in carbon materials such as graphene, carbon nanotubes and carbon fibers; μ' and μ″ in fig. 1 represent real and imaginary parts of permeability, respectively;
FIG. 2 shows the prepared core-shell Fe 3 Reflection loss diagram of C/C fiber composite absorber. The wave absorption performance of the carbon fiber material is characterized by a reflection loss value (RL), and the measured dielectric constant and magnetic permeability are calculated by using a transmission line theory; the diagram is core-shell type Fe 3 The reflection loss diagram of the C/C fiber composite wave absorber is 2-18GHz, and the thickness is 1.00-5.00 mm; in general, when RL is below-10 dB, it indicates that 90% or more of the electromagnetic waves are absorbed, and when RL is below-20 dB, it indicates that 99% or more of the electromagnetic waves are absorbed; as can be seen from the graph, as the thickness of the material increases, the reflection loss peak value moves from high frequency to low frequency, and can be explained by using a 1/4 lambda interference model; core-shell Fe 3 When the thickness of the C/C fiber composite wave absorber is 2.50mm, the maximum reflection loss value is-20.6 dB at 11.52GHz, which shows that the C/C fiber composite wave absorber can absorb more than 99 percent of electromagnetic waves;
FIG. 3 shows the prepared core-shell Fe 3 The wave absorption bandwidth of the C/C fiber composite wave absorber; when RL is lower than-10 dB, more than 90% of electromagnetic waves are absorbed, and the band range of RL < -10dB is called Effective Absorption Bandwidth (EAB); as can be seen from the figure, the prepared core-shell Fe 3 When the thickness of the C/C fiber composite wave absorber is 2.10mm, the effective absorption bandwidth reaches 6.24GHz (11.76 to 18 GHz), and the electromagnetic wave of the Ku wave band (12.88-16.88 GHz) can be completely covered.
Example 2:
core-shell type Fe 3 The preparation method of the C/C fiber composite wave absorber comprises the following steps:
step one, treating polyacrylonitrile powder by adopting low-temperature plasma to obtain pretreated polyacrylonitrile; the low-temperature plasma is dielectric barrier discharge plasma; the conditions for processing the polyacrylonitrile powder by the low-temperature plasma are as follows: in CF 4 In the atmosphere, the current is 2A, the voltage is 110V, and the discharge time is 2min; dissolving pretreated polyacrylonitrile and ferric nitrate in N, N-dimethylformamide, mixing and stirring until the mixture is clear to obtain a mixed solution; the concentration of polyacrylonitrile in the mixed solution is 10wt%; the concentration of ferric nitrate in the mixed solution is 3wt%;
step two, adopting a coaxial spinning stainless steel needle head, and putting the mixed liquid in the step one into a needle cylinder to be used as an external phase; simultaneously taking an iron nitrate solution with the concentration of 5 weight percent as an internal phase; the flow speed is regulated by a micro-injection pump, a direct current power supply is connected to a coaxial spinning stainless steel needle, and coaxial fibers are manufactured by a coaxial electrostatic spinning method; the coaxial electrostatic spinning method comprises the following technological parameters: the flow rate of the external phase microinjection pump is 0.8mL/h, the flow rate of the internal phase microinjection pump is 0.4mL/h, and the flow rate ratio of the internal phase to the external phase is 1:2; the voltage of the direct current power supply is 8kV, and the distance between the coaxial spinning stainless steel needle head and the fiber receiving substrate is 10cm; the coaxial electrostatic spinning is carried out in a constant temperature and humidity box, the temperature is controlled at 20 ℃, and the humidity is controlled at 50%;
step three, the coaxial fibers collected in the step two are put into a muffle furnace, and pre-oxidized in air to obtain pre-oxidized fibers; the pre-oxidation temperature is 300 ℃, the heating rate is 2.5 ℃/min, and the heat preservation time is 2 hours;
step four, placing the pre-oxidized fiber into a tubular furnace, and carbonizing and sintering the pre-oxidized fiber into core-shell Fe in Ar atmosphere 3 C/C doped carbon fiber, i.e. core-shell Fe 3 C/C fiber composite wave absorber; the carbonization temperature of the fiber is 800 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 2 hours; core-shell Fe prepared in this example 3 The C/C fiber composite wave absorber has a maximum reflection loss value of-21.2 dB when the thickness is 2.50 mm.
Example 3:
core-shell type Fe 3 The preparation method of the C/C fiber composite wave absorber comprises the following steps:
step one, treating polyacrylonitrile powder by adopting low-temperature plasma to obtain pretreated polyacrylonitrile; the low-temperature plasma is dielectric barrier discharge plasma; the conditions for processing the polyacrylonitrile powder by the low-temperature plasma are as follows: in CF 4 In the atmosphere, the current is 2A, the voltage is 110V, and the discharge time is 2min; dissolving pretreated polyacrylonitrile and ferric nitrate in N, N-dimethylformamide, mixing and stirring until the mixture is clear to obtain a mixed solution; the concentration of polyacrylonitrile in the mixed solution is 10wt%; the concentration of ferric nitrate in the mixed solution is 3wt%;
step two, adopting a coaxial spinning stainless steel needle head, and putting the mixed liquid in the step one into a needle cylinder to be used as an external phase; simultaneously taking an iron nitrate solution with the concentration of 5 weight percent as an internal phase; the flow speed is regulated by a micro-injection pump, a direct current power supply is connected to a coaxial spinning stainless steel needle, and coaxial fibers are manufactured by a coaxial electrostatic spinning method; the coaxial electrostatic spinning method comprises the following technological parameters: the flow rate of the external phase microinjection pump is 0.8mL/h, the flow rate of the internal phase microinjection pump is 0.4mL/h, and the flow rate ratio of the internal phase to the external phase is 1:2; the voltage of the direct current power supply is 8kV, and the distance between the coaxial spinning stainless steel needle head and the fiber receiving substrate is 10cm; the coaxial electrostatic spinning is carried out in a constant temperature and humidity box, the temperature is controlled at 20 ℃, and the humidity is controlled at 50%;
step three, the coaxial fibers collected in the step two are put into a muffle furnace, and pre-oxidized in air to obtain pre-oxidized fibers; the pre-oxidation temperature is 300 ℃, the heating rate is 2.5 ℃/min, and the heat preservation time is 2 hours;
step four, placing the pre-oxidized fiber into a tubular furnace, and carbonizing and sintering the pre-oxidized fiber into core-shell Fe in Ar atmosphere 3 C/C doped carbon fiber, i.e. core-shell Fe 3 C/C fiber composite wave absorber; the carbonization process is as follows: heating to 300 ℃ at a heating rate of 2.5 ℃/min, preserving heat for 30min, then heating to 800 ℃ at a heating rate of 5 ℃/min, preserving heat for 60min, then heating to 1000 ℃ at a heating rate of 5 ℃/min, and preserving heat for 120min. Core-shell Fe prepared in this example 3 The C/C fiber composite wave absorber has a maximum reflection loss value of-23.5 dB when the thickness is 2.50 mm.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (2)
1. Core-shell type Fe 3 The application of the C/C fiber composite wave absorber in microwave absorption is characterized in that a coaxial mode test is adopted, and core-shell Fe is firstly adopted 3 Grinding the C/C fiber composite wave absorber into powder, mixing with paraffin wax at a ratio of 10wt%, pressing into an annular sample with an inner diameter of 3.04 and mm, an outer diameter of 7.00 and mm and a thickness of 2.00 and mm in a coaxial ring mold, testing the frequency of 2-18GHz, testing the dielectric constant and the magnetic conductivity, and calculating the electromagnetic wave absorption performance of the material by utilizing a transmission line theory;
wherein, the core-shell type Fe 3 The preparation method of the C/C fiber composite wave absorber comprises the following steps:
step one, dissolving polyacrylonitrile and ferric nitrate in an organic solvent, mixing and stirring until the mixture is clear to obtain a mixed solution; the molecular weight of the polyacrylonitrile is 5-15 ten thousand, and the concentration of the polyacrylonitrile in the mixed solution is 3-15 wt%; the concentration of the ferric nitrate in the mixed solution is 0-5 wt%;
step two, adopting a coaxial spinning stainless steel needle head, and putting the mixed liquid in the step one into a needle cylinder to be used as an external phase; taking ferric nitrate solution as an internal phase; the flow speed is regulated by a micro-injection pump, a direct current power supply is connected to a coaxial spinning stainless steel needle, and coaxial fibers are manufactured by a coaxial electrostatic spinning method; the concentration of the ferric nitrate solution is 1-5 wt%;
step three, placing the coaxial fibers collected in the step two into a muffle furnace, and pre-oxidizing in air to obtain pre-oxidized fibers; the pre-oxidation temperature is 280-320 ℃, the temperature rising rate is 1.5-3 ℃/min, and the heat preservation time is 1.5-2.5 h;
step four, placing the pre-oxidized fiber into a tubular furnace, and carbonizing and sintering the pre-oxidized fiber into core-shell Fe in Ar atmosphere 3 C/C doped carbon fiber, i.e. core-shell Fe 3 C/C fiber composite wave absorber; the carbonization process is as follows: heating to 300-450 ℃ at a heating rate of 2.5 ℃/min, preserving heat for 30-60 min, heating to 600-800 ℃ at a heating rate of 5 ℃/min, preserving heat for 30-60 min, heating to 1000-1200 ℃ at a heating rate of 5 ℃/min, and preserving heat for 90-120 min;
in the first step, the polyacrylonitrile is pretreated before use, and the pretreatment process is as follows: treating polyacrylonitrile powder by adopting low-temperature plasma; the low-temperature plasma is dielectric barrier discharge plasma; the conditions for processing the polyacrylonitrile powder by the low-temperature plasma are as follows: in CF 4 Or CCl 4 In the atmosphere, the current is 1.5-2.5A, the voltage is 90-110V, and the discharge time is 1.5-3.5 min;
in the second step, the coaxial electrostatic spinning method comprises the following technological parameters: the flow rate of the external phase microinjection pump is 0.4 mL/h-1 mL/h, the flow rate of the internal phase microinjection pump is 0.2 mL/h-0.5 mL/h, and the flow rate ratio of the internal phase to the external phase is 1:2; the voltage of the direct current power supply is 5 kV-15 kV, and the distance between the coaxial spinning stainless steel needle head and the fiber receiving substrate is 8-12 cm; the coaxial electrostatic spinning is carried out in a constant temperature and humidity box, the temperature is controlled to be 15-25 ℃, and the humidity is controlled to be 40-60%.
2. The core-shell Fe of claim 1 3 The application of the C/C fiber composite wave absorber in microwave absorption is characterized in that in the first step, the organic solvent is N, N-dimethylformamideAmine and/or N-methylpyrrolidone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111003104.4A CN113652769B (en) | 2021-08-30 | 2021-08-30 | Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111003104.4A CN113652769B (en) | 2021-08-30 | 2021-08-30 | Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113652769A CN113652769A (en) | 2021-11-16 |
| CN113652769B true CN113652769B (en) | 2023-08-22 |
Family
ID=78482380
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111003104.4A Active CN113652769B (en) | 2021-08-30 | 2021-08-30 | Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113652769B (en) |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660798A (en) * | 2012-04-28 | 2012-09-12 | 东华大学 | Method for performing coaxial electrostatic blending on polyvinylpyrrolidone(PVP)/chitosan (CS)/Fe3O4 nano fiber film |
| CN103422192A (en) * | 2013-08-05 | 2013-12-04 | 江苏科技大学 | Fe-Co alloy/C composite nanofiber microwave absorbent, and preparation method and application thereof |
| CN103436995A (en) * | 2013-08-05 | 2013-12-11 | 江苏科技大学 | Fe/C composite nanofiber microwave absorbent, preparation method and application of absorbent |
| CN103436994A (en) * | 2013-08-05 | 2013-12-11 | 江苏科技大学 | Fe-Ni alloy/C composite nanofiber microwave absorbent, preparation method and application of absorbent |
| CN104047071A (en) * | 2014-07-07 | 2014-09-17 | 扬州大学 | Preparation method for magnetic active carbon fibers |
| CN105862145A (en) * | 2016-04-19 | 2016-08-17 | 北京化工大学 | Shell-layer-core-layer structure nano composite wave absorbing material and preparation method thereof |
| CN107419365A (en) * | 2017-06-16 | 2017-12-01 | 山东非金属材料研究所 | A kind of graphene composite fibre absorbent and preparation method thereof |
| CN109576823A (en) * | 2018-11-08 | 2019-04-05 | 华南理工大学 | A kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure |
| CN110230129A (en) * | 2019-06-14 | 2019-09-13 | 哈尔滨工业大学 | A kind of surfaces externally and internally growth carbon nanotube contains Fe3Hollow Compound carbon fiber of C and preparation method thereof |
| CN110894624A (en) * | 2019-12-02 | 2020-03-20 | 陕西科技大学 | Magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and preparation method thereof |
| WO2020138552A1 (en) * | 2018-12-27 | 2020-07-02 | 전주대학교산학협력단 | Pan-fe2o3 magnetic composite and manufacturing method therefor |
| CN111850821A (en) * | 2020-06-13 | 2020-10-30 | 北京化工大学 | Method for preparing electromagnetic wave absorbing material from hydrotalcite-based composite nanofiber |
| CN112593312A (en) * | 2020-12-15 | 2021-04-02 | 桐乡市杭福科技有限公司 | Fe3O4-FeCo-carbon nanofiber ternary composite wave-absorbing material and preparation method thereof |
| CN113026148A (en) * | 2021-03-16 | 2021-06-25 | 青岛理工大学 | Magnetic ferrite carbon-based nanofiber wave-absorbing material, preparation method and application |
-
2021
- 2021-08-30 CN CN202111003104.4A patent/CN113652769B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660798A (en) * | 2012-04-28 | 2012-09-12 | 东华大学 | Method for performing coaxial electrostatic blending on polyvinylpyrrolidone(PVP)/chitosan (CS)/Fe3O4 nano fiber film |
| CN103422192A (en) * | 2013-08-05 | 2013-12-04 | 江苏科技大学 | Fe-Co alloy/C composite nanofiber microwave absorbent, and preparation method and application thereof |
| CN103436995A (en) * | 2013-08-05 | 2013-12-11 | 江苏科技大学 | Fe/C composite nanofiber microwave absorbent, preparation method and application of absorbent |
| CN103436994A (en) * | 2013-08-05 | 2013-12-11 | 江苏科技大学 | Fe-Ni alloy/C composite nanofiber microwave absorbent, preparation method and application of absorbent |
| CN104047071A (en) * | 2014-07-07 | 2014-09-17 | 扬州大学 | Preparation method for magnetic active carbon fibers |
| CN105862145A (en) * | 2016-04-19 | 2016-08-17 | 北京化工大学 | Shell-layer-core-layer structure nano composite wave absorbing material and preparation method thereof |
| CN107419365A (en) * | 2017-06-16 | 2017-12-01 | 山东非金属材料研究所 | A kind of graphene composite fibre absorbent and preparation method thereof |
| CN109576823A (en) * | 2018-11-08 | 2019-04-05 | 华南理工大学 | A kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure |
| WO2020138552A1 (en) * | 2018-12-27 | 2020-07-02 | 전주대학교산학협력단 | Pan-fe2o3 magnetic composite and manufacturing method therefor |
| CN110230129A (en) * | 2019-06-14 | 2019-09-13 | 哈尔滨工业大学 | A kind of surfaces externally and internally growth carbon nanotube contains Fe3Hollow Compound carbon fiber of C and preparation method thereof |
| CN110894624A (en) * | 2019-12-02 | 2020-03-20 | 陕西科技大学 | Magnetic metal doped vanadium nitride nano composite fiber microwave absorbent and preparation method thereof |
| CN111850821A (en) * | 2020-06-13 | 2020-10-30 | 北京化工大学 | Method for preparing electromagnetic wave absorbing material from hydrotalcite-based composite nanofiber |
| CN112593312A (en) * | 2020-12-15 | 2021-04-02 | 桐乡市杭福科技有限公司 | Fe3O4-FeCo-carbon nanofiber ternary composite wave-absorbing material and preparation method thereof |
| CN113026148A (en) * | 2021-03-16 | 2021-06-25 | 青岛理工大学 | Magnetic ferrite carbon-based nanofiber wave-absorbing material, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 《Solid and macroporous Fe3》;Huihui Liu等;《SCIENTIFIC REPROTS》;20181115;第8卷;第1-12页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113652769A (en) | 2021-11-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108753251B (en) | ZnO/Co composite nano hollow fiber electromagnetic wave absorbing material and preparation method thereof | |
| CN105219345B (en) | Preparation method of ferroferric oxide @ iron core shell structure-graphene composite absorbing material | |
| CN103422193B (en) | Co/C composite nano fiber microwave absorption, preparation method and application thereof | |
| CN103436994B (en) | Fe-Ni alloy/C/C composite nano fiber microwave absorption, preparation method and application thereof | |
| Guo et al. | The excellent electromagnetic wave absorbing properties of carbon fiber composites: the effect of metal content | |
| CN110177449B (en) | Carbon nanotube-based electromagnetic composite wave-absorbing material and preparation method and application thereof | |
| Jiang et al. | 3D hierarchical porous composites based on natural loofahs/cobalt nanoparticles/graphene oxide with efficient electromagnetic interference shielding performance | |
| CN110042500A (en) | A kind of preparation method of ferroso-ferric oxide/silica composite fiber microwave absorbing material | |
| CN113652769B (en) | Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption | |
| CN110093686A (en) | A kind of TiO2The carbon fibre electromagnetic wave absorbent material and its preparation method and application of/Co load | |
| CN114071982A (en) | Honeycomb reduced graphene oxide foam/nickel nanoparticle wave absorbing agent and preparation method thereof | |
| CN111302324B (en) | Magnetic microporous carbon-based wave-absorbing composite material and preparation method thereof | |
| CN113086965A (en) | Chitosan-based nitrogen-doped carbon aerogel wave-absorbing material and preparation method thereof | |
| CN114752351B (en) | Multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material and preparation method thereof | |
| CN111978742B (en) | Preparation method of carbon fiber wave-absorbing material with dielectric and eddy current losses | |
| CN115216271A (en) | Preparation method of four-shell nitrogen-doped carbon spheres embedded with nano silver particles | |
| CN110947950B (en) | Preparation method of graphene modified FeCo absorbent | |
| CN112391833B (en) | Light high-efficiency wave-absorbing material SnFe 2 O 4 /C composite nanofiber, wave-absorbing coating and preparation method | |
| CN114276781B (en) | MO@NC core-shell structure type nano wave-absorbing material and preparation method thereof | |
| CN115491178B (en) | CoFe (CoFe) 2 O 4 Preparation and application of mesoporous carbon core-shell wave-absorbing material | |
| CN117023555B (en) | Preparation method of hollow carbon/cobalt microsphere wave-absorbing material with graphitization gradient and application of material in wave-absorbing material | |
| CN116322007B (en) | NiFe-CNTs-RGO composite aerogel material with three-dimensional interconnected pore structure, and preparation method and application thereof | |
| CN115160652B (en) | Magnetic nanocellulose-carbon composite aerogel and preparation method and application thereof | |
| CN117468170A (en) | SnO (tin oxide) 2 Composite wave-absorbing material of @ Ni/carbon fiber and preparation method thereof | |
| CN110723723A (en) | Two-dimensional carbon material loaded Fe3N nano-particle light wave-absorbing material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |