CN108753251A - A kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material and preparation method thereof - Google Patents
A kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material and preparation method thereof Download PDFInfo
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- CN108753251A CN108753251A CN201810614095.4A CN201810614095A CN108753251A CN 108753251 A CN108753251 A CN 108753251A CN 201810614095 A CN201810614095 A CN 201810614095A CN 108753251 A CN108753251 A CN 108753251A
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Abstract
The present invention relates to a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent materials and preparation method thereof, are related to electromagnetic wave absorbent material technical field.The method is:1) cobalt source, zinc source are dissolved in DMF, continuously add PVP, is reacted after stirring, obtain uniform tackiness solution;2) it uses high-voltage electrostatic spinning method to carry out spinning to the viscosity solution in step 1), obtains organic nanofibers, will be calcined after organic fiber drying and pre-oxidation treatment;3) will in step 2) being placed in reducing atmosphere after calcining carry out reduction treatment to get.The present invention has the characteristics that saturated magnetization rate is high, coercivity is big, lightweight, oxidation resistance is strong, electromagnetic wave absorption performance is excellent using ZnO/Co composite hollow nano-fiber materials prepared by high-voltage electrostatic spinning method combination calcining reduction, while preparation method is simple, at low cost by the present invention.
Description
Technical field
The present invention relates to electromagnetic wave absorbent material technical field more particularly to a kind of ZnO/Co composite Nanos hollow fibre electricity
Electro-magnetic wave absorption material and preparation method thereof.
Background technology
In recent years, the rapid development of remote sensing, computer technology, electronic communication, also inevitable band
The problems such as having come electromagnetic interference and electromagnetic radiation, meanwhile, increasingly increased electromagnetic energy density causes electromagnetic pollution also to damage
The health of human body.In addition, electromagnetic wave absorbent material also has important application in terms of military technological field.Therefore electromagnetic wave is inhaled
It is of increased attention to receive material, especially for the absorption of the electromagnetic wave of gigahertz frequency range, even more people study
Hot spot.Consider from the loss mechanisms of electromagnetic wave absorbent material, can be mainly divided into electromagnetic wave absorbing material and dielectric absorbing material two
Major class.Traditional electromagnetic wave absorbing material includes ferrite and soft magnetic metal, and domain wall resonance, natural resonance and exchange resonance are
Electromagnetic wave absorbing material dominant loss mechanism.
Typical dielectric absorbing material includes carbon material, conduction high polymer and metal oxide or sulfide, main
Loss mechanisms are interfacial polarization, dipole polarization and electronic polarization etc..According to the matching strip in electro-magnetic wave absorption theory
Part is it is known that if only it is also just to be difficult to obtain excellent it is difficult to meet impedance matching condition to lean on a kind of above-mentioned material
Electromagnetic wave absorption performance.Although the absorbing property of zinc oxide has obtained more in-depth study, zinc oxide is as a kind of
Non-magnetic material can not provide magnetic loss appropriate, thus can not obtain preferable matching effect, which also limits it into one
Step development and application.In order to improve this point deficiency, some researchers combine zinc oxide with magnetic material, and then obtain
Better electromagnetic wave absorption performance.For example document Nanoscale, 2014,6 (12) are prepared for a kind of ZnO/Fe3O4It is compound porous
Ball, and reach absorption maximum when matching thickness is 5mm, maximum reflection loss reaches -40.0dB, also larger upper lift-off
Between.
In addition, the preparation method of existing electromagnetic wave absorbent material is mostly hydro-thermal or the method for solvent heat, experiment is ground
Study carefully, this method is easy to operate, but prepared by the extensive and industrialization that cannot be used for material, thus is unfavorable for practical application and work
Industry produces.In addition, the methods of liquid material exchange method is expensive, and it is cumbersome, also it is suitable only for laboratory research.Therefore, have
Necessity study a kind of zinc oxide electromagnetic wave absorbent material for being conducive to practical application and industrial production and taking into account superperformance and its
Preparation method.
Invention content
For the above-mentioned prior art the problem of, the present invention is intended to provide a kind of ZnO/Co composite Nanos hollow fibre
Electromagnetic wave absorbent material and preparation method thereof.The present invention is multiple using ZnO/Co prepared by high-voltage electrostatic spinning method combination calcining reduction
Conjunction hollow nano fiber material is high with saturated magnetization rate, coercivity is big, lightweight, oxidation resistance are strong, electromagnetic wave absorption performance
Excellent feature, while preparation method is simple, at low cost by the present invention, great industrial applications foreground.
The first object of the present invention is to provide a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material.
The second object of the present invention is to provide a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorb.
The third object of the present invention is to provide a kind of preparation of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material
Method.
The fourth object of the present invention is to provide high-voltage electrostatic spinning method in the preparation of hollow fibre electromagnetic wave absorbent material
Using.
The fifth object of the present invention be to provide ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials and preparation method,
The application of ZnO/Co composite Nano hollow fibre electromagnetic wave absorbs.
For achieving the above object, specifically, the invention discloses following technical proposals:
First, the invention discloses a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material, the electromagnetic waves
Absorbing material is to be stacked to form three-dimensional net structure by one-dimensional hollow nano fiber, and the hollow nano fiber is by ZnO and Co groups
At.
Preferably, in the electromagnetic wave absorbent material, the molar ratio of ZnO and Co are 1:1;And Co is face-centred cubic structure,
ZnO is close-packed hexagonal structure.
Preferably, in the electromagnetic wave absorbent material, the outer diameter of hollow nano fiber is 200-300nm.
Preferably, in the electromagnetic wave absorbent material, hollow nano fiber wall thickness is 20-40nm.
Preferably, the saturated magnetization rate of the electromagnetic wave absorbent material is 31.15emu/g.
Preferably, the coercivity H of the electromagnetic wave absorbent materialcFor 480.5Oe.
Secondly, the invention discloses a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorb, the absorber by
ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials and paraffin mixed configuration prepared by the present invention forms.
Preferably, the mass ratio of the electromagnetic wave absorbent material and paraffin is 1:1.
Preferably, the absorber matching thickness is 3.0mm, and frequency reaches absorption maximum intensity when being 11.4GHz, anti-
It is -68.4dB to penetrate loss.
Preferably, the absorber is under single matching thickness, when matching thickness is 2.6mm, effective absorption band width
For 5.9GHz, effective absorption band width refers to:Electro-magnetic wave absorption RL<- 10dB, i.e., 90% electromagnetic wave are absorbed.
Again, the invention discloses a kind of preparation method of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material,
Include the following steps:
(1) with acetylacetone cobalt (II) (C10H14O4) or cobalt nitrate (Co (NO Co3)2·9H2) and two water zinc acetates O
C4H6O4Zn·2H2O is raw material, provides electrospun solution viscosity with polyvinylpyrrolidone (PVP), uses n,N-Dimethylformamide
(DMF) it is used as solvent;Acetylacetone cobalt or cobalt nitrate and zinc acetate are dissolved in DMF, PVP is continuously added, is reacted after stirring,
Obtain uniform tackiness solution;
(2) it uses high-voltage electrostatic spinning method to carry out spinning to the viscosity solution in step (1), obtains organic nanofibers,
It will be calcined after organic fiber drying and pre-oxidation treatment;
(3) product after calcining in step (2) is placed in reducing atmosphere carry out reduction treatment to get.
In step (1), the acetylacetone cobalt or cobalt nitrate, two water zinc acetates, DMF, PVP adding proportion be 1mmol:
1-3mmol:10ml:1-1.5g preferably 1mmol:1mmol:10ml:1.5g.
In step (1), the temperature of the reaction is 500-600 DEG C, reaction time 3-5h.
In step (2), the voltage of the high-voltage electrostatic spinning method is 10-15kV.
In step (2), the drying temperature and time are:30-80℃,12-24h.
In step (2), the pre-oxidation treatment is:1-4h is kept the temperature at 150-300 DEG C.
In step (2), the calcination temperature is 400-700 DEG C, time 3-5h.
In step (3), the reducing atmosphere is hydrogen.
In step (3), the holding temperature is 200-400 DEG C, time 1-3h.
In step (3), the reduction treatment carries out in closed tube furnace.
Finally, the invention also discloses ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials and preparation method thereof,
ZnO/Co composite Nano hollow fibre electromagnetic wave absorbs are micro- in radio communication system, anti-high frequency, microwave heating equipment, construction
Application in wave darkroom, stealth technology.
It should be noted that metallic cobalt have higher saturated magnetization rate and the Snoek limit, with zinc oxide it is compound after have
Conducive to the better chemical stability of acquisition and saturated magnetization rate performance;In addition, in addition to the intrinsic matching properties of material to be considered and
Outside drain performance, microstructure and particle size, form etc. can also have an important influence on the electromagnetic wave absorption performance of material,
And hollow-core construction is capable of providing the specific surface area and better dispersibility of bigger, improves being in direct contact for electromagnetic wave and absorbing material
Area, this can be more advantageous to the absorption of electromagnetic wave.At the same time, hollow-core construction can effectively introduce air, reduce the opposite of material
Dielectric constant is conducive to the impedance matching performance for improving material;
And high-voltage electrostatic spinning apparatus is relatively easy, it is easy to operate, controllability is strong, and actual industrial production is had been used to,
Therefore, the present invention prepares the solid nanofiber with one-dimensional microstructure using high-voltage electrostatic spinning, and constructs three with this
Solid nanofiber can be changed into hollow nanofiber, such microcosmic knot by dimension network in conjunction with subsequent heat treatment mode
Structure is capable of providing the specific surface area of bigger, the loss of the conductance of long-range, and is conducive to the multipath reflection and multiple scattering of electromagnetic wave,
Be conducive to further increasing for electromagnetic wave absorption performance.
The principle of the present invention is:First, it is electrostatic spinning process, when the electric field force being applied in liquid solution is more than solution
When the surface tension of itself, solution can be pulled out under the action of electric field force by anode, fly to cathode;And PVP exists for solution
Increasing viscosity so that solution is not broken up in drawing process as droplet, but adhesion is at silk, and with volatile molten
Agent DMF can volatilize in nano wire flight course, finally obtain solid nanofiber and received by cathode.Thus obtain second
The compound organic nanofibers of acyl acetone cobalt or cobalt nitrate, zinc acetate, PVP three.
Secondly, it is the formation of hollow-core construction, this has benefited from the atomic diffusion process under Kinkendal Effect driving:Organic
In the calcination process of nanofiber, since the diffusion velocity of oxygen in the fibre is less than the diffusion speed of metal ion (cobalt, zinc)
Degree, therefore metal ion is diffused into fibrous outer and is combined to form metal oxide with oxygen, at the same time, PVP is also constantly
By oxygenolysis, to which organic nanofibers are finally changed into oxide (zinc oxide, cobaltosic oxide) nano-hollow fiber.
Finally, it is reduction process, hydrogen is reduced to metallic cobalt as reducing agent, by cobaltosic oxide, and zinc oxide cannot
It is reduced, it is final to obtain ZnO/Co composite hollow nanofibers.
Compared with prior art, the advantageous effect that the present invention obtains is:
(1) ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials prepared by the present invention have excellent impedance matching
Performance and unique microscopic appearance, and it can also can keep being suitble to magnetic conductivity in the range in high frequency, have very excellent
Electromagnetic wave absorption performance.
(2) hollow-core construction has the characteristics that lightweight, therefore the ZnO/Co composite Nanos hollow fibre electricity prepared with the present invention
Electro-magnetic wave absorption material can prepare the thin electromagnetic wave absorb of lightweight, thickness.
(3) preparation process of the invention is simple, does not need complicated hardware device, environmentally safe, low manufacture cost,
It is very suitable for industrial production.
(4) fibre dimensions of ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials prepared by the present invention are uniform, resist
Oxidation and corrosion resistance are strong.
(5) the saturated magnetization rate of ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials prepared by the present invention reaches
31.15emu/g coercivity HcUp to 480.5Oe;The matter of ZnO/Co composite hollows nanofiber and paraffin in manufactured absorber
Amount is than being 1:When 1, manufactured absorber is 3.0mm in matching thickness, and frequency reaches absorption maximum intensity when being 11.4GHz,
Reflection loss is -68.4dB;Under single matching thickness, when matching thickness is 2.6mm, effective absorption band width is reachable
5.9GHz。
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not constitute the improper restriction to the application for explaining the application.
Fig. 1 is gained ZnO/Co after embodiment 1 is calcined3O4The XRD diffracting spectrums and ZnO/ of composite hollow nano-fiber material
The XRD diffracting spectrums of Co composite hollow nanofiber electromagnetic wave absorbent materials.
Fig. 2 is the SEM figures of organic nanofibers prepared by embodiment 1.
Fig. 3 is the SEM figures of ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials prepared by embodiment 1.
Fig. 4 is the TEM figures of ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials prepared by embodiment 1.
Fig. 5 is that the magnetism testing of ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials prepared by embodiment 1 is bent
Line.
Fig. 6 is ZnO/Co composite hollow nanofiber electromagnetic wave absorbent material electro-magnetic wave absorption curves prepared by embodiment 1.
Fig. 7 is the electro-magnetic wave absorption curve of ZnO hollow nano fiber electromagnetic wave absorbent materials prepared by comparative example 1.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
As background technology is introduced, the preparation method of existing electromagnetic wave absorbent material is mostly hydro-thermal or solvent heat
Method, for experimental study, this method is easy to operate, but cannot be used for material extensive and industrialization prepare, because without
Conducive to practical application and industrial production, and the methods of liquid material exchange method is expensive, cumbersome, is also suitable only for laboratory
Research, therefore, the present invention propose a kind of utilization electrostatic spinning process preparation ZnO/Co composite Nano hollow fibre electromagnetic waves suction
The method for receiving material, the present invention is described further with reference to the accompanying drawings and detailed description.
In the embodiment of the present invention, with acetylacetone cobalt (II) (C10H14O4) or cobalt nitrate (Co (NO Co3)2·9H2O), two water
Zinc acetate (C4H6O4Zn·2H2O) it is respectively cobalt source, zinc source, electrospun solution viscosity is provided with polyvinylpyrrolidone (PVP), with
N,N-dimethylformamide (DMF) is used as solvent.
Embodiment 1
A kind of preparation method of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material, includes the following steps:
(1) 1mmol acetylacetone cobalts and bis- water zinc acetates of 1mmol are fully added after dissolving by being dissolved in 10ml DMF
Enter 1.5g PVP, react 3h after stirring at 600 DEG C, obtains uniform tackiness solution;
(2) under the conditions of 12kV high-pressure electrostatics, the viscosity solution in step (1) is spun with high-voltage electrostatic spinning technique
Silk, obtains organic fiber, then by organic fiber in 50 DEG C of dry 20h, then is placed in sky after pre-oxidation treatment 3h at 200 DEG C
In the Muffle furnace of gas atmosphere, 3h is calcined at 600 DEG C;
(3) product after calcining in step (2) is placed in closed tube furnace, in hydrogen atmosphere, is kept the temperature at 400 DEG C
1h carries out reduction treatment to get ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials.
Comparative example 1
With embodiment 1, difference lies in:Cobalt source acetylacetone cobalt (II) is not added.
Embodiment 2
With embodiment 1, difference lies in:In step (1), with cobalt nitrate (Co (NO3)2·9H2O acetylacetone cobalt) is substituted
(II)(C10H14O4Co).In step (2), drying time and temperature are:30℃,24h;The time of pre-oxidation treatment and temperature are:
300 DEG C of pre-oxidation treatment 1h.
Embodiment 3
With embodiment 1, difference lies in:In step (1), the additive amount of the PVP is 1.0g.In step (2), drying time
It is with temperature:80℃,12h;The time of pre-oxidation treatment and temperature are:150 DEG C of pre-oxidation treatment 4h.
Embodiment 4
With embodiment 1, difference lies in:In step (1), the additive amount of the two water zinc acetate is 2mmol.In step (2),
Drying time and temperature are:70℃,20h;The time of pre-oxidation treatment and temperature are:250 DEG C of pre-oxidation treatment 2h.
Embodiment 5
With embodiment 1, difference lies in:In step (1), the temperature of the reaction is 500 DEG C, reaction time 5h.Step
(2) in, the voltage of the high-voltage electrostatic spinning method is 10kV, and the calcination temperature is 700 DEG C, time 3h.In step (3),
The holding temperature is 200 DEG C, time 3h.
Embodiment 6
With embodiment 1, difference lies in:In step (1), the additive amount of the two water zinc acetate is 3mmol, the reaction
Temperature be 550 DEG C, reaction time 4h.In step (2), the voltage of the high-voltage electrostatic spinning method is 15kV, the calcining
Temperature is 400 DEG C, time 5h.In step (3), the holding temperature is 300 DEG C, time 2h.
Performance test:
XRD tests are carried out to ZnO/Co composite Nano hollow fibre electromagnetic wave absorbent materials prepared by embodiment 1, as a result such as
Shown in Fig. 1, show the oxidation of the metallic cobalt containing body-centered cubic structure and hexagonal structure in ZnO/Co composite hollow nanofibers
Zinc, and compared with standard diffraction data (JCPDS-150806) and (JCPDS-361451) and show that the iron purity of synthesis is very high.
The organic nanofibers prepared to embodiment 1 are observed in the secure execution mode (sem, and the results are shown in Figure 2, it can be seen that:It is organic to receive
Rice fibre diameter is about 450nm, and is solid fibre.
The ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials prepared to embodiment 1 are observed at SEM and TEM,
As a result as shown in Figures 3 and 4, it can be seen that:The nanofiber crossed after hydrogen reducing is hollow-core construction, wall thickness 20-40nm it
Between, outer diameter is between 200-300nm.
With the magnetism for the ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials that VSM magnetometers prepare embodiment 1
It can be tested, the results are shown in Figure 5, it can be seen that:Saturated magnetization rate is 31.15emu/g, coercivity HcUp to 480.5Oe.
ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials prepared by embodiment 1 are with paraffin according to mass ratio 1:
It is pressed into cricoid absorber sample (D after 1 ratio mixingOutside×dIt is interior× h=7 × 3.04 × 2.0mm), there is related parameter εrAnd μrWith
Agilent Technologies E8363A electromagnetic wave vector network analyzers measure, and reflection loss is by εr、μr, absorption frequency and
The thickness of sample determines that the electro-magnetic wave absorption curve of absorber is as shown in Figure 6, it can be seen that εr' ranging from 2-18GHz, value
Between 5.4-9.2.εr" in 10.0GHz, 14.0GHz and 15.2GHz, there are three formants respectively.μr' and μr" variation range point
Not Wei 0.91-1.14 and 0-0.21, absorption peak minimum value is -68.4dB, and absorptivity is less than the bandwidth of -10dB under single thickness
For 5.9GHz.
ZnO hollow nano fibers electromagnetic wave absorbent material prepared by comparative example 1 is with paraffin according to mass ratio 1:1 ratio
Cricoid absorber sample (D is pressed into after mixingOutside×dIt is interior× h=7 × 3.04 × 2.0mm), related parameter εrAnd μrUse Agilent
Technologies E8363A electromagnetic wave vector network analyzers measure, and reflection loss is by εr、μr, absorption frequency and sample thickness
Degree determines that the electro-magnetic wave absorption curve of absorber is as shown in Figure 7, it can be seen that its electromagnetic wave absorption performance is deteriorated, effective band
Narrow.And XRD is the results show that the ZnO/Co composite hollow nanofiber electromagnetic wave absorbent materials prepared are the oxygen of hexagonal structure
Change zinc, due to not containing magnetisable material, the impedance matching performance of material is deteriorated, and electromagnetic wave absorption performance is deteriorated, and effective band becomes
It is narrow, it is unfavorable for the absorption of electromagnetic wave.
The foregoing is merely the preferred embodiments of the application, are not intended to limit this application, for those skilled in the art
For member, the application can have various modifications and variations.Any modification made by within the spirit and principles of this application,
Equivalent replacement, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. application of the high-voltage electrostatic spinning method in the preparation of hollow fibre electromagnetic wave absorbent material.
2. a kind of preparation method of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material, it is characterised in that:The method
Include the following steps:
(1) using acetylacetone cobalt (II) or cobalt nitrate and two water zinc acetates as raw material, it is molten to provide electrospinning with polyvinylpyrrolidone
Fluid viscosity uses n,N-Dimethylformamide as solvent;Acetylacetone cobalt or cobalt nitrate and zinc acetate are dissolved in DMF, after
It is continuous that PVP is added, it is reacted after stirring, obtains uniform tackiness solution;
(2) it uses high-voltage electrostatic spinning method to carry out spinning to the viscosity solution in step (1), obtains organic nanofibers, will have
It is calcined after machine fiber drying and pre-oxidation treatment;
(3) will in step (2) being placed in reducing atmosphere after calcining carry out reduction treatment to get.
3. preparation method as claimed in claim 2, it is characterised in that:In step (1), the acetylacetone cobalt or cobalt nitrate,
Two water zinc acetates, DMF, PVP adding proportion be 1mmol:1-3mmol:10ml:1-1.5g preferably 1mmol:1mmol:
10ml:1.5g;
Or, in step (1), the temperature of the reaction is 500-600 DEG C, reaction time 3-5h;
Or, in step (2), the drying temperature and time are:30-80℃,12-24h;
Or, in step (2), the pre-oxidation treatment is:1-4h is kept the temperature at 150-300 DEG C;
Or, in step (2), the voltage of the high-voltage electrostatic spinning method is 10-15kV;
Or, in step (2), the calcination temperature is 400-700 DEG C, time 3-5h.
4. preparation method as claimed in claim 2 or claim 3, it is characterised in that:In step (3), the reducing atmosphere is hydrogen;
Or, in step (3), the holding temperature is 200-400 DEG C, time 1-3h;
Or, in step (3), the reduction treatment carries out in closed tube furnace.
5. a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material, it is characterised in that:The electromagnetic wave absorbent material
To stack the three-dimensional net structure formed by one-dimensional hollow nano fiber, the hollow nano fiber is made of ZnO and Co,
In, Co is face-centred cubic structure, and ZnO is close-packed hexagonal structure.
6. electromagnetic wave absorbent material as claimed in claim 5, it is characterised in that:The outer diameter of the hollow nano fiber is 200-
The wall thickness of 300nm, hollow nano fiber are 20-40nm, and in electromagnetic wave absorbent material, and the molar ratio of ZnO and Co are 1:1.
7. such as electromagnetic wave absorbent material described in claim 5 or 6, it is characterised in that:The saturation of the electromagnetic wave absorbent material
Magnetic susceptibility is 31.15emu/g, coercivity HcFor 480.5Oe.
8. a kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorb, the absorber is by electromagnetic wave absorbent material and paraffin
Mixed configuration forms, it is characterised in that:The electromagnetic wave absorbent material is prepared by claim 2-4 any one of them methods
Electromagnetic wave absorbent material and/or claim 5-7 any one of them electromagnetic wave absorbent materials.
9. electromagnetic wave absorb as claimed in claim 8, it is characterised in that:The quality of the electromagnetic wave absorbent material and paraffin
Than being 1:1;
Or, the absorber matching thickness is 3.0mm, frequency reaches absorption maximum intensity, reflection loss when being 11.4GHz
For -68.4dB;
Or, the absorber, under single matching thickness, when matching thickness is 2.6mm, effective absorption band width is 5.9GHz.
10. such as claim 2-4 any one of them method and/or such as claim 5-7 any one of them electro-magnetic wave absorptions
Material and/or absorber as claimed in claim 8 or 9 are in radio communication system, anti-high frequency, microwave heating equipment, construction
Application in microwave dark room, stealth technology.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101792170A (en) * | 2010-02-10 | 2010-08-04 | 长春理工大学 | Method for preparing cerium dioxide polycrystal nanobelt |
CN105702937A (en) * | 2016-04-08 | 2016-06-22 | 扬州大学 | Preparation method of SnO2/C fiber |
CN106400205A (en) * | 2016-11-21 | 2017-02-15 | 江南大学 | Preparation method of hollow magnetic iron oxide nanofiber |
CN106519854A (en) * | 2016-12-02 | 2017-03-22 | 济南大学 | Magnetic sterilizing heat-insulation coating and preparation method thereof |
-
2018
- 2018-06-14 CN CN201810614095.4A patent/CN108753251B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101792170A (en) * | 2010-02-10 | 2010-08-04 | 长春理工大学 | Method for preparing cerium dioxide polycrystal nanobelt |
CN105702937A (en) * | 2016-04-08 | 2016-06-22 | 扬州大学 | Preparation method of SnO2/C fiber |
CN106400205A (en) * | 2016-11-21 | 2017-02-15 | 江南大学 | Preparation method of hollow magnetic iron oxide nanofiber |
CN106519854A (en) * | 2016-12-02 | 2017-03-22 | 济南大学 | Magnetic sterilizing heat-insulation coating and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
LI-YUAN FAN,等: "ZnO@Co hybrid nanotube arrays growth from electrochemical deposition: structural, optical, photocatalytic and magnetic properties", 《PHYS. CHEM. CHEM. PHYS》 * |
ZENGYONG CHU,等: "Effects of diameter and hollow structure on the microwave absorption properties of short carbon fibers", 《CERAMICS INTERNATIONAL》 * |
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CN111389403A (en) * | 2020-03-24 | 2020-07-10 | 福州大学 | Zn/Co doped carbon material and preparation method and application thereof |
CN111389403B (en) * | 2020-03-24 | 2022-11-15 | 福州大学 | Zn/Co doped carbon material and preparation method and application thereof |
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