CN104927762B - Class worm hole porous carbon/magnetic particle composite wave-absorbing agent and preparation method thereof - Google Patents
Class worm hole porous carbon/magnetic particle composite wave-absorbing agent and preparation method thereof Download PDFInfo
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- CN104927762B CN104927762B CN201510292093.4A CN201510292093A CN104927762B CN 104927762 B CN104927762 B CN 104927762B CN 201510292093 A CN201510292093 A CN 201510292093A CN 104927762 B CN104927762 B CN 104927762B
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- magnetic particle
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Abstract
One species worm hole porous carbon/magnetic particle composite wave-absorbing agent and preparation method thereof, belongs to electromagnetic wave absorbent material technical field.It is by the cobalt doped ferroso-ferric oxide particle of polyacrylonitrile and coated with silica according to certain ratio by solution blending by way of mix, obtain polyacrylonitrile/magnetic particle solution；Solution is coated on glass plate, fast transfer is into water, and immersion, taking-up obtains polyacrylonitrile/magnetic particle porous composite film after air drying；Obtained polyacrylonitrile/magnetic particle porous composite film is pre-oxidized at a certain temperature, is carbonized, grinding is obtained with class worm hole porous carbon/magnetic particle composite wave-absorbing agent.Wherein, the mass ratio of porous carbon and magnetic particle is 75~85：25~15, a diameter of 40~100nm of class worm hole.Graphite multi-walled carbon nano-tube/Nanocomposites the wave absorbing agent prepared using the present invention, further using paraffin as matrix, can prepare the absorbing material of different wave absorbing agent loadings.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material technical field, more particularly to a species worm hole porous carbon/magnetic
Particle composite wave-absorbing agent and preparation method thereof.
Background technology
In recent years, with the fast development of electronics industry, electromagnetic pollution is on the rise, and absorbing material is anti-in electromagnetic pollution
Protector for collar domain serves vital effect.Realizing the radar invisible of military equipment simultaneously, weakening electromagnetic interference, guarantee information
The fields such as safety, absorbing material has also played particularly important effect.Absorbing material (microwave absorbing material, electromagnetic wave attenuation material
Material or Radar Stealth Materials) reflection of the electromagnetic wave in body surface can be efficiently reduced, while so that inciding material internal
Electromagnetic wave be efficiently damped.Absorbing material can be divided into wave absorbing agent and matrix according to its composition.Matrix is in absorbing material
Cohesive effect is primarily served, and wave absorbing agent is the main body of absorbing material, plays a part of electromagnetic wave loss.Outstanding wave absorbing agent
Need to meet lightweight, absorption intensity are big, absorption band is wide, electromagnetic consumable ability is strong and environmental resistance it is strong in terms of need
Ask.
Carbon material, with good chemical stability, excellent heat endurance, high mechanical strength and outstanding electric conductivity
Advantage in terms of energy.The light weight of carbon material, has larger potentiality in the wave absorbing agent field for preparing outstanding simultaneously.However,
According to transmission line theory (Qin, F.；Brosseau, C., J.Appl.Phys.2012,111,061301), for one-component
Wave absorbing agent (dielectric loss type or magnetic loss type), due to being difficult to the matching of preferable electromagnetic parameter in same material, so
The final absorbing property of material is limited, and the requirement of efficient absorbing material, lightweight and wideband, therefore system can not have been met gradually
The standby composite wave-absorbing agent for having dielectric loss and magnetic loss concurrently, two kinds of losses are effectively combined, current absorbing material is had become and grinds
Study carefully the focus in field.Composite wave-absorbing agent has relatively good electromagnetic matching ability, can efficiently reduce electromagnetic wave and inhale ripple
The reflection of material surface so that electromagnetic wave can be effectively entered inside absorbing material, passes through the dielectric loss and magnetic of material
Loss, electromagnetic wave is effectively absorbed, and obtains excellent absorbing property, more and more important angle is play in absorbing material field
Color.However, the introducing of magnetic material, often make it that the wave absorbing agent prepared has larger density, this is for mitigating absorbing material
Quality be unfavorable.So, the focus being designed to for nowadays lightweight absorbing material research field of porous absorbing material.Together
When, the introducing of loose structure can effectively increase the contact probability of electromagnetic wave and wave absorbing agent so that electromagnetic wave and wave absorbing agent
Interaction increase, can most incident electromagnetic wave be fast and effeciently lost at last.Therefore, ripple material is being inhaled in porous composite wave-absorbing agent
Material field plays more and more important role.
The content of the invention
The invention provides a kind of excellent class worm hole porous carbon/magnetic particle composite wave-absorbing agent of absorbing property and its
Preparation method.The preparation technology of the composite wave-absorbing agent is simple, is easy to operation, it is easy to produce, at the same the material prepared have it is porous
Structure, its absorbing property is excellent, with wider suction wave frequency band, stronger absorption intensity, the characteristic such as lightweight, in absorbing material neck
Domain has larger application potential.In the present invention, using polyacrylonitrile as matrix, the magnetic particle of coated with silica is passed through
In the method for solution blending, incorporation polyacrylonitrile, porous polypropylene nitrile/magnetic particle is prepared by the method for inversion of phases and is combined
Film, obtained composite membrane has been obtained by pre-oxidation, carbonization and grinding there is class worm hole porous carbon/magnetic particle to be combined
Wave absorbing agent.The wave absorbing agent absorbing property of preparation is excellent, show C-band (4~8GHz) for electromagnetic wave, X-band (8~
12GHz) and KuThe stronger absorption of wave band (12~18GHz), its maximum reflection loss has reached that (Fig. 6 can reflect -36dB
Go out).
Class worm hole porous carbon/magnetic particle composite wave-absorbing agent provided by the present invention, porous carbon and magnetic particle
Mass ratio is 75~85：25~15, (this some holes is all through hole, hole and hole to a diameter of 40~100nm of class worm hole
Between be also connection).
The preparation process of composite wave-absorbing agent is divided into three below step：By polyacrylonitrile and the cobalt doped of coated with silica
Ferroso-ferric oxide particle is mixed according to certain ratio by way of solution blending, obtains polyacrylonitrile/magnetic particle solution；
Solution is coated on glass plate, fast transfer is into water, and immersion, taking-up obtains polyacrylonitrile/magnetic after air drying
Particle porous composite film；Obtained polyacrylonitrile/magnetic particle porous composite film is pre-oxidized at a certain temperature, is carbonized, is ground
Mill is obtained with class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
The preparation method of class worm hole porous carbon/magnetic particle composite wave-absorbing agent of the present invention, its specific step
It is rapid as follows：
(1) under nitrogen protection, into 150~250mL distilled water, add 5~6mmol ferric chloride hexahydrates, 2.0~
2.5mmol Iron dichloride tetrahydrates and 0.4~0.6mmol cobalt chloride hexahydrates, warming-in-water are added to 60~80 DEG C thereto
Concentrated ammonia liquor (mass percent 25~28%) is 9~11 to pH, continues to react 30~90min, Magneto separate is reclaimed, by recovery product
Using respectively washing 5~8 times of distilled water and absolute ethyl alcohol, it is scattered in 5~15mL distilled water；Dispersion liquid is added to 200~
Added in 400mL ethanol, at 30~50 DEG C 5~7mL distilled water, 7~9mL concentrated ammonia liquors (mass percent 25~28%), 0.8~
1.2mL tetraethyl orthosilicates, react 9~11h；Magneto separate is reclaimed, by recovery product using distilled water and absolute ethyl alcohol respectively washing 5~
8 times, 60~90 DEG C of dry 10~15h in vacuum drying oven are subsequently placed in, the cobalt doped ferroso-ferric oxide of coated with silica is obtained
Particle；
(2) the cobalt doped ferroso-ferric oxide particle of 0.25~0.40g coated with silica is used into 12~16mL dimethyl
Formamide (DMF or dimethylacetylamide, because dissolubility is just only in strong solvent for the polyacrylonitrile used below
It is good) 1~3h of ultrasonic disperse, add 2.0~3.0g polyacrylonitrile, 0.1~0.2g PVPs, 50~70 DEG C of heating
1~3h is dissolved, solution is poured on the flat board of surfacing, 12~36h, air after taking-up is soaked after knifing in distilled water
Middle 12~36h of drying, obtains polyacrylonitrile/magnetic particle porous composite film；
(3) polyacrylonitrile of preparation/magnetic particle porous composite film is heated into 3~6h at 200~300 DEG C, so
0.5~2h of carbonization treatment under 900~1100 DEG C of vacuum again, obtains porous carbon/magnetic particle composite membrane afterwards, and composite membrane is abundant
Grinding, obtains class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
Using graphite multi-walled carbon nano-tube/Nanocomposites wave absorbing agent for preparing of the present invention, further using paraffin as
Matrix, can prepare the absorbing material of different wave absorbing agent loadings, and the method that it is prepared is as follows：
(1) paraffin and class worm hole porous carbon/magnetic particle composite wave-absorbing agent are mixed, the matter of wave absorbing agent in mixture
It is 25%~35% to measure percentage composition；
(2) it is that 7mm, internal diameter are 3mm that the mixture for obtaining step (1) is suppressed into external diameter by mould using hydraulic press
Test annulus；Thickness 2mm；
(3) electromagnetic parameter of the above-mentioned obtained sample in the range of 2~18GHz is tested using Agilent N5244A PNA-X
(ε ', ε ", μ ', μ "), reflection loss RL (Lu Shaowei, Li Qian, the Xiong Xuhai, horse of the composite wave-absorbing agent are calculated using following formula
Gram bright, Xu Weikai, Jia Caixia, Journal of Inorganic Materials, 2015,30,23-28).
In formula：Z0It is free space impedance (by μ0、ε0Calculated using formula)；μ0、ε0It is that space permeability and dielectric are normal
Number, ε0=8.854187817 × 10-12F/m, μ0=4 π × 10-7H/m；ZinBe absorbing material input impedance (utilize ε ', ε ",
μ ', μ " data calculation)；F is the frequency of electromagnetic wave (scope is 2~18GHz)；D is the thickness of absorbing material；C is electromagnetic wave
In the spread speed of free space, equal to the light velocity 3 × 108m/s；εr(εr=ε '-j ε ") and μr(μr=μ '-j μ ") it is absorbing material
Equivalent relative complex dielectric constant and complex permeability, j is the imaginary part unit of complex dielectric constant and complex permeability, no reality
Border meaning.Experiment can measure ε ', ε ", μ ', μ " of the material under different wave frequency f.
Brief description of the drawings
Fig. 1：The cobalt doped ferroso-ferric oxide particle and class of coated with silica prepared by embodiment 1 and embodiment 2 are compacted
Worm channel hole porous carbon/magnetic particle composite wave-absorbing agent XRD spectra.
Fig. 2：The stereoscan photograph of porous carbon/magnetic particle composite membrane prepared by embodiment 2, illustration is composite membrane office
Portion's enlarged drawing.
Fig. 3：The stereoscan photograph of class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared by embodiment 2, is inserted
Figure is composite wave-absorbing agent partial enlargement electromicroscopic photograph.
Fig. 4：The hole diameter distribution of the class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared in embodiment 2
Figure.
Fig. 5：The energy spectrum analysis datagram of class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared by embodiment 2.
Fig. 6：The electromagnetic parameter meter for the class worm hole porous carbon/magnetic particle composite wave-absorbing agent tested using embodiment 3
Obtained reflection loss RL datagrams.
The ferroso-ferric oxide particle and class worm hole that Fig. 1 gives the cobalt doped of the coated with silica of preparation are porous
The XRD spectra of carbon/magnetic particle composite wave-absorbing agent, analysis of spectra understands that the cobalt doped four of the coated with silica of preparation is aoxidized
The purity of three iron particles is higher, and carbon crystallinity is relative in obtained class worm hole porous carbon/magnetic particle composite wave-absorbing agent
Smaller, this unformed structure can bring active influence for the polarization in the electric field of material, and four oxygen of cobalt doped
The diffraction maximum for changing three-iron disappears substantially, the diffraction maximum for iron and cobalt nanometer particle of appearance, illustrates four oxidations three of cobalt doped
Iron is reduced to cobalt simple substance and iron simple substance at high temperature, and this change also can the absorbing property final to material bring certain
Influence.
What Fig. 2 was provided is the photo of the ESEM of the porous carbon/magnetic particle composite membrane prepared, from the photograph of ESEM
As can be seen that obtained composite membrane has obvious finger pore structure in piece, and its cell walls is then shown as with class worm hole
The nano pore structure of hole structure.
What Fig. 3 was provided is the stereoscan photograph of ground obtained composite wave-absorbing agent in embodiment 2, passes through electromicroscopic photograph
It was found that, by grinding, finger hole destruction, and the nano-pore with class worm pore space structure on duct is kept, and this
The work of transmission path of the electromagnetic wave inside wave absorbing agent, increase electromagnetic wave and wave absorbing agent can effectively be increased by planting porous structure
With to realizing that the good absorption to electromagnetic wave has certain facilitation.
Fig. 4 gives the hole diameter of the class worm hole porous carbon/magnetic particle composite wave-absorbing agent prepared in embodiment 2
The statistics of size, from statistics knowable to, the size distribution of worm hole between 40~100nm, and 70nm proportion most
Greatly.
Fig. 5 gives the energy spectrum analysis number of class worm hole porous carbon/magnetic particle composite wave-absorbing agent of the preparation of embodiment 2
According to, it is known that, in the composite wave-absorbing agent of preparation, the content of carbon is 79.2%, and magnetic component content is 20.8%.
Fig. 6 gives the data that the reflection loss RL that obtained electromagnetic parameters are obtained is tested using embodiment 3.From
Understood in figure, material shows stronger electromaganic wave absorbing property.When thickness is 1.5mm, material is shown to electromagnetism
Ripple KuWave band preferably absorbs, and frequency bandwidths of the RL less than -10dB has reached 4GHz.Continue to increase the thickness of wave absorbing agent, inhale
Receive peak to be moved to electromagnetic wave low frequency direction, the characteristic for still keeping wideband to absorb.When the thickness of wave absorbing agent reaches 4.0mm,
Material shows the characteristic of biabsorption frequency band, C-band and K that can simultaneously to electromagnetic waveuWave band shows stronger suction
Receive.Therefore, the material of preparation has wideband, thin matching thickness, the characteristic absorbed by force concurrently, shows C-band to electromagnetic wave, X
Wave band and KuThe stronger absorbability of wave band.
Embodiment
Embodiment 1：
The synthetic method of the cobalt doped Fe 3 O 4 magnetic particle for the coated with silica that the present invention is provided, can by with
Lower reactions steps are realized：
(1) under nitrogen protection, into 200mL distilled water, 5.4mmol ferric chloride hexahydrates, the water of 2.16mmol tetra- are added
Frerrous chloride and 0.54mmol cobalt chloride hexahydrates are closed, warming-in-water is to 70 DEG C；
(2) it is 10 to add concentrated ammonia liquor (mass percent 25~28%) thereto to pH, continues to react 60min, product magnetic
Separation and recovery, by recovery product using distilled water and absolute ethyl alcohol respectively washing 6 times, is scattered in 10mL distilled water；
(3) dispersion liquid is added in 300mL ethanol, 6mL distilled water, 8mL concentrated ammonia liquor (mass percents is added at 40 DEG C
25~28%), 1.0mL tetraethyl orthosilicates react 10h；Product uses Magneto separate, uses distilled water and absolute ethyl alcohol respectively washing 6
Time, 70 DEG C of dry 12h in vacuum drying oven are subsequently placed in, the cobalt doped ferroso-ferric oxide particle of coated with silica is obtained.
Embodiment 2：
The synthetic method for class worm hole porous carbon/magnetic particle composite wave-absorbing agent that the present invention is provided, can be by following
Reactions steps are realized：
(1) the cobalt doped ferroso-ferric oxide particle of 0.32g coated with silica is super using 14mL dimethylformamides (DMF)
Sound disperses 2h, adds 2.4g polyacrylonitrile, 0.16g PVPs, 60 DEG C of heating for dissolving 2h；
(2) solution is poured on glass plate, using blade applicator knifing, is transferred to the container for filling a large amount of distilled water
In, 24h, air drying 24h after taking-up are soaked, polyacrylonitrile/magnetic particle porous composite film is obtained；
(3) polyacrylonitrile of preparation/magnetic particle porous composite film is transferred in high temperature oven, 250 DEG C of heating
4h；
(4) film after processing is transferred in high temperature process furnances, 1000 DEG C of vacuum carburizations handle 1h, obtain porous carbon/
Magnetic particle composite membrane, composite membrane is fully ground, and obtains class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
Embodiment 3：
The application of graphite multi-walled carbon nano-tube/Nanocomposites wave absorbing agent prepared as the present invention, using paraffin as
Matrix, is prepared for the test sample of different wave absorbing agent loadings, can be realized by following steps：
(1) paraffin and class worm hole porous carbon/magnetic particle composite wave-absorbing agent are mixed according to certain mass ratio；
Wherein the mass percent of wave absorbing agent/(wave absorbing agent+paraffin) is 30%；
(2) by the mixture of the wave absorbing agent of upper step and paraffin by mould using hydraulic press be suppressed into external diameter for 7mm,
Internal diameter is the test annulus that 3mm, thickness are 2mm；
(3) electromagnetic parameter of the above-mentioned obtained sample in the range of 2~18GHz is tested using Agilent N5244A PNA-X
(ε ', ε ", μ ', μ "), the reflection loss RL of the composite wave-absorbing agent is calculated using formula.
Claims (5)
1. the preparation method of a species worm hole porous carbon/magnetic particle composite wave-absorbing agent, its step is as follows：
(1) under nitrogen protection, into 150~250mL distilled water, add 5~6mmol ferric chloride hexahydrates, 2.0~
2.5mmol Iron dichloride tetrahydrates and 0.4~0.6mmol cobalt chloride hexahydrates, warming-in-water are added to 60~80 DEG C thereto
Concentrated ammonia liquor is 9~11 to pH, continues to react 30~90min, Magneto separate is reclaimed, and recovery product is used into distilled water and absolute ethyl alcohol
It is each to wash 5~8 times, it is scattered in 5~15mL distilled water；Dispersion liquid is added in 200~400mL ethanol, at 30~50 DEG C
5~7mL distilled water, 7~9mL concentrated ammonia liquors, 0.8~1.2mL tetraethyl orthosilicates are added, 9~11h is reacted；Magneto separate is reclaimed, and will be returned
Product is received using distilled water and absolute ethyl alcohol respectively washing 5~8 times, 60~90 DEG C of dry 10~15h in vacuum drying oven are subsequently placed in,
Obtain the cobalt doped ferroso-ferric oxide particle of coated with silica；
(2) the cobalt doped ferroso-ferric oxide particle of 0.25~0.40g coated with silica is used into 12~16mL dimethyl formyls
Amine or dimethylacetylamide, 1~3h of ultrasonic disperse add 2.0~3.0g polyacrylonitrile, 0.1~0.2g polyvinylpyrrolidones
Ketone, 50~70 DEG C of 1~3h of heating for dissolving, solution is poured on the flat board of surfacing, 12 are soaked after knifing in distilled water
12~36h of air drying after~36h, taking-up, obtains polyacrylonitrile/magnetic particle porous composite film；
(3) polyacrylonitrile of preparation/magnetic particle porous composite film is heated into 3~6h, Ran Houzai at 200~300 DEG C
0.5~2h of carbonization treatment under 900~1100 DEG C of vacuum, obtains porous carbon/magnetic particle composite membrane, composite membrane is fully ground
Mill, obtains class worm hole porous carbon/magnetic particle composite wave-absorbing agent.
2. a species worm hole porous carbon/magnetic particle composite wave-absorbing agent, it is characterised in that：It is as described in claim 1
Method is prepared；In carbonisation, magnetic ferrites are reduced to iron cobalt nanometer particle, class worm hole be through hole and
It is connection, a diameter of 40~100nm of class worm hole between hole and hole.
3. species worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 2, it is characterised in that：It is many
The ratio of hole carbon and magnetic particle is 75~85：15~25.
4. species worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 2, it is characterised in that：Enter
One step prepares the absorbing material of different composite wave absorbing agent loading by matrix of paraffin.
5. species worm hole porous carbon/magnetic particle composite wave-absorbing agent as claimed in claim 4, it is characterised in that：It is
Paraffin and class worm hole porous carbon/magnetic particle composite wave-absorbing agent are sufficiently mixed uniformly, wherein the quality of composite wave-absorbing agent
Percentage composition is 25%~35%.
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| CN106495680B (en) * | 2016-11-08 | 2019-04-05 | 太原科技大学 | The sheet calcium hexaluminate microwave absorbing ceramic compound material preparation method of carried magnetic metal simple-substance |
| CN106520071B (en) * | 2016-12-06 | 2018-05-25 | 吉林大学 | Rice husk base carbon/magnetism Co particle composite wave-absorbing agent and preparation method thereof |
| CN107835625B (en) * | 2017-09-18 | 2020-06-02 | 浙江理工大学 | Porous sheet cobalt/carbon composite wave-absorbing material and preparation method thereof |
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| CN103131384B (en) * | 2013-02-28 | 2014-06-04 | 湖南大学 | Nanometer composite wave absorbing powder having low density and porous structure, and its preparation method |
| CN103864408B (en) * | 2014-03-27 | 2015-04-01 | 北京理工大学 | Ferrite nano-pore microsphere wave-absorbing material and preparation method thereof |
| CN104446417A (en) * | 2014-12-04 | 2015-03-25 | 浙江大学 | Porous block-shaped ferrite prepared based on loofah sponge and preparation method of porous block-shaped ferrite |
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