CN117691367A - Electromagnetic shielding wave-absorbing material C/MoS 2 Preparation method and application thereof - Google Patents
Electromagnetic shielding wave-absorbing material C/MoS 2 Preparation method and application thereof Download PDFInfo
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Abstract
An electromagnetic shielding wave-absorbing material, which is cotton fiber derived C/MoS 2 The composite material, specifically, is prepared into biomass-derived tubular carbon fiber by taking cotton fiber as a raw material, and then MoS is deposited on the surface of the biomass-derived tubular carbon fiber by hydrothermal deposition 2 Form MoS 2 C/MoS for wrapping tubular carbon fiber 2 A composite structure. The material has excellent electromagnetic wave shielding performance, has lower reflection loss value of-41.7 dB in the frequency range of 2-18 GHz, and the electromagnetic wave shielding wave absorbing material C/MoS prepared by the invention 2 Can be applied to lifeAnd various equipment and products needing electromagnetic shielding in the work, such as shale gas exploitation equipment, mining machinery equipment and the like, medical instruments and aerospace equipment, so that the interference of electromagnetic waves on the normal work of the equipment is reduced, and in addition, the equipment can be used in military equipment, and the shielding function is realized by absorbing the electromagnetic waves.
Description
Technical Field
The invention relates to electromagnetic shielding technologyThe technical field, in particular to an electromagnetic shielding wave-absorbing material C/MoS 2 And a preparation method and application thereof.
Background
The wave absorbing material is a functional material capable of absorbing electromagnetic waves in space, and can convert electromagnetic wave radiation into heat energy or other forms of energy to be consumed, so that the reflection intensity of the electromagnetic waves on the surface of the material is reduced. In engineering application, the wave absorbing material is required to have light weight, heat resistance, moisture resistance, corrosion resistance and the like besides high absorptivity of electromagnetic waves in a wider frequency band. With the development of modern science and technology, in airports, aircraft flights cannot take off due to electromagnetic wave interference; in hospitals, mobile phones often interfere with the proper operation of various electronic medical instruments. In addition, various weaponry and military facilities are coated with absorbing materials, so that the absorbing materials can absorb the reconnaissance electric waves and attenuate the reflected signals, thereby breaking through the defense area of the enemy radar, being a powerful means of anti-radar reconnaissance, the rapid development of radar detection technology brings forward higher technical requirements on the electromagnetic wave stealth performance of the military equipment, and also brings forward the performance requirements on the used absorbing materials for light weight, high reinforcement and wide frequency. On the other hand, electromagnetic radiation problems are common in household appliances and various operation equipment nowadays, electromagnetic radiation causes direct and indirect harm to human bodies through thermal effects, non-thermal effects and accumulation effects, and increasingly serious electromagnetic radiation pollution problems also affect the health of human bodies and the reliability of precision electronic equipment. Therefore, high-performance light electromagnetic wave absorbing materials are in urgent need in both military and civilian industries.
The carbon-based nano material has the advantages of light weight and easiness in compounding with other materials, and is one of hot spots for researching the wave-absorbing material. The carbon-based nano wave-absorbing material has a plurality of types, wherein the biomass-derived carbon material can better retain the morph-genetic structure of the carbonized natural raw material, and is beneficial to improving the electromagnetic wave loss capability of the material in the special structural forms of an ordered pore structure, a hollow tubular structure, a hierarchical structure and the like. The natural cotton fiber is in a one-dimensional hollow tubular structure and consists of a plurality of concentric layers from outside to inside, has a nearly circular cross-sectional shape, has simple material composition,the biomass-derived carbon source mainly contains cellulose, water and trace organic matters, and is very suitable for being used as a biomass-derived carbon source. However, pure cotton fiber derived carbon has poor impedance matching, and a single electromagnetic wave loss mechanism, which cannot meet the requirements of practical application. In order to optimize the wave absorbing performance, composite components can be introduced to design and regulate the microstructure of the composite material. Nanometer molybdenum disulfide (MoS) 2 ) The material is a typical two-dimensional material, has good response to electromagnetic waves, has ultra-thin thickness and ultra-large specific surface area, and can be used as an impedance matching regulator to be compounded with cotton fiber derived carbon materials, so that the aim of improving impedance matching and wave absorbing performance is fulfilled.
Disclosure of Invention
The invention aims to provide an electromagnetic shielding wave-absorbing material C/MoS 2 。
Another object of the present invention is to provide the electromagnetic shielding wave-absorbing material C/MoS 2 Is prepared by the preparation method of (1). Solves the problem of preparing MoS by hydrothermal method 2 The technical problems of agglomeration and uneven wrapping occur, and the wave absorbing performance of the material is effectively improved.
A third object of the present invention is to provide an electromagnetic shielding wave-absorbing material C/MoS 2 Is used in the application of (a).
The invention aims at realizing the following technical scheme:
an electromagnetic shielding wave absorbing material, which is characterized in that: the wave-absorbing material is cotton fiber derived C/MoS 2 The composite material, specifically, is prepared into biomass-derived tubular carbon fiber by taking cotton fiber as a raw material, and then MoS is deposited on the surface of the biomass-derived tubular carbon fiber by hydrothermal deposition 2 Form MoS 2 And a composite structure wrapping the tubular carbon fibers.
Further, the preparation of biomass-derived tubular carbon fiber is to take absorbent cotton balls, heat treat the absorbent cotton balls in an inert atmosphere at 600-800 ℃ for 5-6 h to obtain the tubular carbon fiber with cotton fiber genetic structure.
Further, the hydrothermal deposition MoS 2 Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolve inDissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature.
Further, sodium molybdate dihydrate, CH in the mixed solution 4 N 2 The dosage of S and deionized water is 1-2 mmol:4-8 mmol:30mL, and the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL.
Further, after the hydrothermal reaction is finished, centrifuging for 2min at a rotation speed of 8000r/min, separating a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material.
Electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) is characterized in that: preparing biomass-derived tubular carbon fiber by taking cotton threads as raw materials, and performing hydrothermal deposition MoS on the surface of the biomass-derived tubular carbon fiber 2 Form MoS 2 C/MoS for wrapping tubular carbon fiber 2 The preparation of the biomass-derived tubular carbon fiber is to take absorbent cotton balls, perform heat treatment under inert atmosphere, and obtain the tubular carbon fiber with cotton fiber genetic structure, wherein the heat treatment temperature is 600-800 ℃ and the heat preservation time is 5-6 h.
Further, the hydrothermal deposition MoS 2 Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature.
Further, sodium molybdate dihydrate, CH in the mixed solution 4 N 2 The dosage of S and deionized water is 1-2 mmol:4-8 mmol:30mL, and the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL.
Further, after the hydrothermal reaction is finished, centrifuging for 2min at a rotation speed of 8000r/min, separating a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 Drying oven for removing impurities through O multiple times of cleaning at 60 DEG CMedium drying for 24h to obtain cotton fiber derived C/MoS 2 A composite material.
Most specifically, an electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) is characterized by comprising the following steps:
(1) Taking absorbent cotton balls, drying the absorbent cotton balls in a vacuum environment, and then performing heat treatment in an inert atmosphere at 600-800 ℃ for 5-6 hours to obtain tubular carbon fibers with cotton fiber morph-genetic structures;
(2) Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature, wherein sodium molybdate dihydrate and CH are contained in the mixed solution 4 N 2 S and deionized water are used in an amount of 1-2 mmol: 4-8 mmol:30mL, the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL;
(3) After the thermal reaction is finished, centrifuging for 2min at 8000r/min, separating out a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material.
Electromagnetic shielding wave-absorbing material C/MoS prepared by the method 2 The application in preparing wave-absorbing paint.
An electromagnetic shielding wave-absorbing coating is characterized in that: comprises a resin material and a wave-absorbing material C/MoS 2 A coupling agent, a dispersing agent, an anti-settling agent, a plasticizer and a solvent, wherein the wave-absorbing material C/MoS 2 Preparing biomass-derived tubular carbon fibers by taking cotton fibers as raw materials, and then performing hydrothermal deposition of MoS on the surfaces of the biomass-derived tubular carbon fibers 2 Form MoS 2 C/MoS for wrapping tubular carbon fiber 2 A composite structure.
Further, the preparation of biomass-derived tubular carbon fiber is to take absorbent cotton balls, heat treat the absorbent cotton balls in an inert atmosphere at 600-800 ℃ for 5-6 h to obtain the tubular carbon fiber with cotton fiber genetic structure.
Further, the hydrothermal deposition MoS 2 Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature.
Further, sodium molybdate dihydrate, CH in the mixed solution 4 N 2 The dosage of S and deionized water is 1-2 mmol:4-8 mmol:30mL, and the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL.
Further, after the hydrothermal reaction is finished, centrifuging for 2min at a rotation speed of 8000r/min, separating a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material.
The preparation process finds that the molybdenum disulfide is easy to generate agglomeration phenomenon in the hydrothermal growth process, and the wave absorbing performance of the prepared composite material is not ideal.
In the preparation process, cotton fibers are firstly prepared into biomass-derived tubular carbon fibers and then added into a hydrothermal reaction system, the carbon fibers inherit the natural tubular structure of raw materials, and can form a steric hindrance effect in a solution in a hydrothermal environment, so that MoS is inhibited 2 The stacking and agglomeration of the nano-sheets further improves the specific surface area of the material, generates more active sites, and simultaneously the carbon fiber is MoS 2 Growth during hydrothermal processes provides nucleation sites such that MoS 2 The nano-sheets can grow and cover the surfaces of the carbon fibers to form uniform and complete packages for the tubular carbon fibers.
Molybdenum disulfide synthesized by a hydrothermal method on the surface of cotton fiber biomass derived tubular carbon fiber has the characteristics of abundant defects and many surface dangling bonds, induced electrons in the molybdenum disulfide move along a molecular network to form dissipation current, good response to electromagnetic waves is achieved, and the combined hollow tubular carbon fiber inside the molybdenum disulfide is incidentThe electromagnetic wave provides a longer transmission channel, and the combination of the two can increase the multiple scattering and multiple absorption of the electromagnetic wave in the cavity, and the one-dimensional tubular structure has high specific surface area and high defect density, can generate more space charge polarization and dipole polarization, accelerates the circulation of electrons, and improves the conductivity loss of the material. The two components are grown in situ and self-assembled to obtain C/MoS 2 The composite material can improve the impedance matching characteristic of the composite material, adjust electromagnetic parameters and increase heterogeneous interface polarization loss, thereby improving the wave absorbing performance of the composite material.
By adjusting the proportion of molybdenum atoms and carbon atoms in the hydrothermal process, the C/MoS can be changed 2 The wave-absorbing properties of the composite material were found by continuous attempts to adjust C/MoS 2 When the mole ratio of molybdenum to carbon atoms in the composite material is 1.5:10, the broadband high-strength wave-absorbing material can be obtained.
Further, the resin material is obtained by mixing epoxy resin and acrylic resin according to a ratio of 1:1.
Further, the coupling agent is a titanate coupling agent, the dispersing agent comprises at least one of polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol and propylene carbonate, the anti-settling agent comprises at least one of bentonite, polyamide wax and polyethylene wax, the plasticizer comprises at least one of dibutyl phthalate (DBP) and dioctyl phthalate (DOP), and the solvent can be at least one of ethanol, n-butanol, isopropanol, ethyl acetate, acetone or deionized water.
Further, the coating comprises the following components in parts by weight:
40-45 parts of resin material and C/MoS 2 30-40 parts of coupling agent, 2-4 parts of dispersing agent, 1-2 parts of dustproof agent, 0.5-1 part of plasticizer, 1-1.5 parts of solvent and 35-45 parts of solvent.
Further preferably, the amount of each component in the coating is 40 parts of resin material, C/MoS 2 35 parts of coupling agent, 3 parts of dispersing agent, 1.5 parts of dust-proof agent, 0.6 part of plasticizer, 1.2 parts of solvent and 40 parts of solvent.
The preparation method of the electromagnetic shielding wave-absorbing coating is characterized by comprising the following steps:
(1) C/MoS of wave-absorbing material 2 Adding a coupling agent into a solvent for ultrasonic dispersion to obtain a mixed solution A, wherein the ultrasonic power is 800-1000W, and the ultrasonic time is 20-40 min;
(2) And adding the resin material, the plasticizer, the dispersing agent and the anti-settling agent into the mixed solution A for high-speed stirring and dispersing, wherein the stirring speed is 1500-2500 rpm, and the stirring time is 1-1.5 h.
The invention has the following technical effects:
the invention prepares the electromagnetic shielding wave-absorbing material C/MoS through the participation of cotton-thread derived carbon fibers 2 The electromagnetic wave shielding material can efficiently absorb electromagnetic waves and achieve the effect of shielding the electromagnetic waves, has lower reflection loss value in the frequency range of 2-18 GHz, is-41.7 dB, has large effective wave absorption width in the thickness range of 1.0-5.0 mm, has the effective wave absorption width of 12.32GHz, particularly 5.68-18GHz, and has excellent electromagnetic wave shielding performance, and the electromagnetic wave shielding wave absorbing material C/MoS prepared by the invention has the advantages of low cost, high energy consumption, low cost and low cost 2 The electromagnetic shielding device can be applied to various equipment and products requiring electromagnetic shielding in life and work, such as shale gas exploitation equipment, mining machinery equipment and the like, and medical instruments, communication equipment and aerospace equipment, so that interference of electromagnetic waves on normal work of the equipment is reduced.
Drawings
Fig. 1: biomass-derived C/MoS prepared in example 1 2 Is a scanning electron microscope image of (1).
Fig. 2: comparative example 1 prepared C/MoS 2 Is a scanning electron microscope image of (1).
Fig. 3: biomass derived C/MoS prepared in example 1 2 Is a reflectance graph of (2).
Fig. 4: comparative example 1 prepared C/MoS 2 Is a reflectance graph of (2).
Fig. 5: example 2 preparation of Biomass derived C/MoS 2 Is a reflectance graph of (2).
Fig. 6: example 3 preparation of Biomass derived C/MoS 2 Is a reflectance graph of (2).
Detailed Description
The present invention is described in detail below by way of examples, which are necessary to be pointed out herein for further illustration of the invention and are not to be construed as limiting the scope of the invention, since numerous insubstantial modifications and adaptations of the invention will be to those skilled in the art in light of the foregoing disclosure.
Example 1
Electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) comprises the following steps:
(1) Taking absorbent cotton balls, drying in a vacuum environment, and then performing heat treatment in an inert atmosphere, wherein the heat treatment temperature is 700 ℃, and the heat preservation time is 5.5 hours to obtain tubular carbon fibers with cotton fiber morph-genetic structures;
(2) Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 200 ℃ for 24 hours, and cooling to room temperature, wherein the dosage of sodium molybdate dihydrate, thiourea and deionized water in the mixed solution is 1.5 mmol/6 mmol/30 mL, and the dosage ratio of the tubular carbon fibers to the mixed solution is 1 mmol/3 mL;
(3) After the thermal reaction is finished, centrifuging for 2min at 8000r/min, separating out a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material having a molybdenum/carbon atom molar ratio of 1.5:10.
As can be seen from fig. 1, the biomass-derived carbon generated by carbonizing the cotton fiber well maintains the fiber structure, and the MoS grows on the surface of the carbon fiber in situ 2 Nanoplatelets, moS 2 Uniformly distributed on the surface of the carbon fiber and self-assembled to form C/MoS 2 The composite material improves the impedance matching characteristic of the composite material, adjusts electromagnetic parameters and increases heterogeneous interface polarization loss, thereby improving the wave absorbing performance of the composite material.
By preparingThe obtained C/MoS 2 The composite material is mixed with paraffin wax, and the electromagnetic performance of the composite material is tested by adopting a coaxial method, specifically, a sample to be tested and the paraffin wax are mixed according to a certain filling proportion, and then the mixture is placed in a coaxial mould, and the mixture is pressed into a coaxial circular ring with the inner diameter of about 3mm, the outer diameter of about 7mm and the thickness of about 2 mm. The coaxial ring is placed in a coaxial line clamp and is connected with two coaxial line ports of the vector network analyzer through a connector. The excitation signal sent by the signal source of the network vector analyzer is equally divided into two paths of signals through a signal separator, one path of signals enters a receiver to be tested and is used as a reference signal, the other path of signals are extracted by a directional coupler, finally, the amplitude and the phase of the two paths of signals are obtained through a processing display unit, the scattering parameter sum of the wave-absorbing material in the frequency range of 2.0-18.0 GHz is obtained, the transmission coefficient and the reflection coefficient are obtained through the scattering parameter, the electromagnetic parameter of the wave-absorbing material is further determined, and after the dielectric constant and the magnetic conductivity are obtained, the reflection values of the sample at different frequencies are calculated according to a related formula. As a result, as shown in FIG. 3, C/MoS was measured at a coating thickness of 4.5mm 2 The lowest reflection loss value was-41.7 dB. The effective wave absorption width is 12.32GHz within the thickness range of 1.0-5.0 mm, and the effective absorption of more than 95% of electromagnetic waves within the range of 5.68-18GHz can be realized.
Comparative example 1
C/MoS 2 The preparation method of (2) comprises the following steps:
(1) Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, dispersing absorbent cotton balls into fibers, adding the fibers into the mixed solution, stirring and mixing, carrying out hydrothermal reaction at 200 ℃ for 24 hours, and cooling to room temperature, wherein the dosage of sodium molybdate dihydrate, thiourea and deionized water in the mixed solution is 1.5 mmol/6 mmol/30 mL;
(2) Centrifuging at 8000r/min for 2min after hydrothermal reaction, separating product obtained by hydrothermal reaction, and adding deionized water and C 2 H 6 O is cleaned for many times to remove impurities and then is dried for 24 hours in a drying oven at 60 ℃ to obtain C/MoS 2 A precursor;
(3) C/MoS 2 The precursor is put into inert atmosphere for heat treatment, the heat treatment temperature is 700 ℃, and the heat preservation time is 5.5h to obtain C/MoS 2 。
In comparative example 1, moS was first formed on the surface of cotton fiber 2 The greatest problem in the preparation process is that the C/MoS can not be improved by regulating and controlling the proportion of molybdenum to carbon atoms 2 The purpose of the wave absorbing performance of the material is that the cotton fiber which is not carbonized in the hydrothermal process cannot be MoS 2 Nucleation provides more attachment points, thus MoS 2 The coating effect on the surface of the fiber is poor, C/MoS 2 More heterostructures cannot be formed in the composite material and MoS is not possible due to steric hindrance 2 Significant agglomeration occurred, which adversely affected the wave absorbing properties as shown in FIG. 2, and it can be seen from FIG. 4 that the C/MoS prepared in comparative example 1 2 The lowest reflection loss value of the (C) is-12.5 dB, and the effective wave-absorbing width is 10.5GHz in the thickness range of 1.0-5.0 mm.
In the preparation process, we also tried to directly use other tubular carbon fiber materials (non-cotton fiber biomass derived carbon fibers) for preparing C/MoS 2 Composite material, but the performance of the prepared composite material is not C/MoS prepared by taking cotton fiber as raw material 2 The composite material has excellent performance.
Example 2
Electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) comprises the following steps:
(1) Taking absorbent cotton balls, drying in a vacuum environment, and then performing heat treatment in an inert atmosphere, wherein the heat treatment temperature is 800 ℃, and the heat preservation time is 5 hours to obtain tubular carbon fibers with cotton fiber morph-genetic structures;
(2) Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190 ℃ for 22 hours, and cooling to room temperature, wherein sodium molybdate dihydrate and CH in the mixed solution 4 N 2 S and deionized water are used in an amount of 1mmol:4mmol:30mL, and the ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL;
(3) After the thermal reaction is finished, centrifuging for 2min at 8000r/min, separating out a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material having a molybdenum/carbon atom molar ratio of 1:10.
As shown in FIG. 5, at a coating thickness of 5mm, C/MoS 2 The minimum reflection loss value is-33.6 dB, the effective wave absorption width is 12.3GHz within the thickness range of 1.0-5.0 mm, and the effective absorption of 95% of electromagnetic waves within the range of 5-18GHz can be realized.
Example 3
Electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) comprises the following steps:
(1) Taking absorbent cotton balls, drying in a vacuum environment, and then performing heat treatment in an inert atmosphere, wherein the heat treatment temperature is 600 ℃, and the heat preservation time is 6 hours to obtain tubular carbon fibers with cotton fiber morph-genetic structures;
(2) Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 210 ℃ for 20 hours, and cooling to room temperature, wherein sodium molybdate dihydrate and CH (CH) are contained in the mixed solution 4 N 2 S and deionized water are used in an amount of 2mmol, 8mmol and 30mL, and the ratio of the tubular carbon fiber to the mixed solution is 1mmol, 3mL;
(3) After the thermal reaction is finished, centrifuging for 2min at 8000r/min, separating out a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material having a molybdenum/carbon molar ratio of 1:5.
As a result, as shown in FIG. 3, C/MoS was measured at a coating thickness of 4.5mm 2 The minimum reflection loss value is41.7dB, and the effective wave absorption width is 12.32GHz in the thickness range of 1.0-5.0 mm.
As shown in FIG. 6, at a coating thickness of 5mm, C/MoS 2 The minimum reflection loss value is-28.6 dB, the effective wave absorption width is 12.7GHz within the thickness range of 1.0-5.0 mm, and the effective absorption of 95% of electromagnetic waves within the range of 5-18GHz can be realized.
Example 4
Magnetic shielding wave-absorbing material C/MoS prepared in example 1 2 The preparation method for the wave-absorbing paint comprises the following steps:
(1) The wave-absorbing material C/MoS prepared in example 1 2 Adding a coupling agent into a solvent for ultrasonic dispersion to obtain a mixed solution A, wherein the ultrasonic power is 1000W, and the ultrasonic time is 30min;
(2) Adding a resin material, a plasticizer, a dispersing agent and an anti-settling agent into the mixed solution A for high-speed stirring and dispersing, wherein the stirring speed is 1500rpm, and the stirring time is 1.5h;
the amount of each component in the paint is 40 parts of resin material and C/MoS 2 35 parts of coupling agent, 1.5 parts of dispersing agent, 0.6 part of dustproof agent, 1.2 parts of plasticizer and 40 parts of solvent, wherein the resin material is formed by mixing epoxy resin and acrylic resin according to a volume ratio of 1:1, the coupling agent is titanate coupling agent, the dispersing agent is polyvinylpyrrolidone, the anti-settling agent is polyethylene wax, the plasticizer is dibutyl phthalate (DBP), and the solvent is ethanol and isopropanol according to a volume ratio of 1:1.
Example 5
Magnetic shielding wave-absorbing material C/MoS prepared in example 2 2 The preparation method for the wave-absorbing paint comprises the following steps:
(1) The wave-absorbing material C/MoS prepared in example 2 2 Adding a coupling agent into a solvent for ultrasonic dispersion to obtain a mixed solution A, wherein the ultrasonic power is 900W, and the ultrasonic time is 20min;
(2) Adding a resin material, a plasticizer, a dispersing agent and an anti-settling agent into the mixed solution A for high-speed stirring and dispersing, wherein the stirring speed is 2500rpm, and the stirring time is 1h;
the resin material is formed by mixing epoxy resin and acrylic resin according to a ratio of 1:1, wherein the coupling agent is titanate coupling agent, the dispersing agent is polyethylene glycol, the anti-settling agent is bentonite, the plasticizer is dioctyl phthalate (DOP), the solvent is ionized water, and the weight portion of each component in the coating is 45 portions of the resin material and C/MoS 2 40 parts of a coupling agent, 4 parts of a dispersing agent, 2 parts of a dust-proof agent, 1.5 parts of a plasticizer and 45 parts of a solvent.
Example 6
Magnetic shielding wave-absorbing material C/MoS prepared in example 2 2 The preparation method for the wave-absorbing paint comprises the following steps:
(1) The wave-absorbing material C/MoS prepared in example 3 2 Adding a coupling agent into a solvent for ultrasonic dispersion to obtain a mixed solution A, wherein the ultrasonic power is 800W, and the ultrasonic time is 40min;
(2) And adding a resin material, a plasticizer, a dispersing agent and an anti-settling agent into the mixed solution A for high-speed stirring and dispersing, wherein the stirring speed is 1800rpm, and the stirring time is 1h.
The resin material is formed by mixing epoxy resin and acrylic resin according to a ratio of 1:1, wherein the coupling agent is titanate coupling agent, the dispersing agent is polyvinyl alcohol, the anti-settling agent is polyethylene wax, the plasticizer is dibutyl phthalate (DBP), and the solvent is ethyl acetate; the coating comprises the following components in parts by mass:
the resin material is 42 parts, C/MoS 2 30 parts of coupling agent, 1 part of dispersing agent, 0.5 part of dust-proof agent, 1 part of plasticizer and 35 parts of solvent.
The performance of the wave-absorbing coating prepared in examples 4 to 6 was tested by a vector network analyzer in a microwave darkroom by adopting a reflectivity bow measurement method, the test angle is 15 degrees, the test range is 2 to 18GHz, and the test is carried out by referring to GJB 2038-1994, the test method for reflectivity of radar wave-absorbing material, and the results are shown in Table 1.
Table 1:
| corresponding coating | bandwidth/GHz less than or equal to-10 dB | Minimum reflection loss | Corresponding frequency/GHz |
| Example 4 | 5.4 | -40.3 | 10.4 |
| Example 5 | 5.2 | -31.4 | 8.9 |
| Example 6 | 4.6 | -26.5 | 11.2 |
It can be seen that the cotton fiber biomass prepared by the present invention was derived from C/MoS 2 After the paint is prepared, the wave absorbing performance of the paint is kept at a higher level.
Claims (8)
1. An electromagnetic shielding wave absorbing material, which is characterized in that: the wave-absorbing material is cotton fiber derived C/MoS 2 The composite material, specifically, is prepared into biomass-derived tubular carbon fiber by taking cotton fiber as a raw material, and then MoS is deposited on the surface of the biomass-derived tubular carbon fiber by hydrothermal deposition 2 Form MoS 2 C/MoS for wrapping tubular carbon fiber 2 A composite structure.
2. An electromagnetically shielded wave-absorbing material as claimed in claim 1, wherein: the preparation of biomass derived tubular carbon fiber is to take absorbent cotton balls, heat treat the absorbent cotton balls in inert atmosphere at 600-800 ℃ for 5-6 h to obtain the tubular carbon fiber with cotton fiber morph-genetic structure.
3. An electromagnetic shielding wave absorbing material according to claim 1 or 2, wherein: the hydrothermal deposition MoS 2 Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature.
4. An electromagnetic shielding wave absorbing material according to any one of claims 1-3, wherein: sodium molybdate dihydrate, CH in the mixed solution 4 N 2 The dosage of S and deionized water is 1-2 mmol:4-8 mmol:30mL, and the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL.
5. Electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) is characterized in that: preparing biomass-derived tubular carbon fiber by taking cotton threads as raw materials, and performing hydrothermal deposition MoS on the surface of the biomass-derived tubular carbon fiber 2 Form MoS 2 C/MoS for wrapping tubular carbon fiber 2 The preparation of the biomass-derived tubular carbon fiber is to take absorbent cotton balls, perform heat treatment under inert atmosphere, and obtain the tubular carbon fiber with cotton fiber genetic structure, wherein the heat treatment temperature is 600-800 ℃ and the heat preservation time is 5-6 h.
6. An electromagnetic shielding wave-absorbing material C/MoS as defined in claim 5 2 The preparation method of (2) is characterized in that: the hydrothermal deposition MoS 2 Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature.
7. An electromagnetic shielding wave-absorbing material C/MoS as defined in claim 5 or 6 2 The preparation method of (2) is characterized in that: sodium molybdate dihydrate, CH in the mixed solution 4 N 2 The dosage of S and deionized water is 1-2 mmol:4-8 mmol:30mL, and the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL.
8. Electromagnetic shielding wave-absorbing material C/MoS 2 The preparation method of (2) is characterized by comprising the following steps:
(1) Taking absorbent cotton balls, drying the absorbent cotton balls in a vacuum environment, and then performing heat treatment in an inert atmosphere at 600-800 ℃ for 5-6 hours to obtain tubular carbon fibers with cotton fiber morph-genetic structures;
(2) Sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in deionized water to form a mixed solution, adding tubular carbon fibers, stirring and mixing, performing hydrothermal reaction at 190-210 ℃ for 20-24 h, and cooling to room temperature, wherein sodium molybdate dihydrate and CH are contained in the mixed solution 4 N 2 The dosage of S and deionized water is 1-2 mmol:4-8 mmol:30mL, and the dosage ratio of the tubular carbon fiber to the mixed solution is 1mmol:3mL;
(3) After the thermal reaction is finished, centrifuging for 2min at 8000r/min, separating out a product obtained by the hydrothermal reaction, and using deionized water and C 2 H 6 O is dried for 24 hours in a drying oven at 60 ℃ after the impurities are removed by multiple times of cleaning, and the cotton fiber derived C/MoS is obtained 2 A composite material.
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| CN112063365A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| CN116084158A (en) * | 2023-02-20 | 2023-05-09 | 中国科学院长春应用化学研究所 | Biomass-based FeS particle composite fiber, preparation method thereof and electromagnetic absorption material |
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