CN105062417B - A kind of organo-mineral complexing nanometer microwave absorbing material and preparation method thereof - Google Patents
A kind of organo-mineral complexing nanometer microwave absorbing material and preparation method thereof Download PDFInfo
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- CN105062417B CN105062417B CN201510416495.0A CN201510416495A CN105062417B CN 105062417 B CN105062417 B CN 105062417B CN 201510416495 A CN201510416495 A CN 201510416495A CN 105062417 B CN105062417 B CN 105062417B
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Abstract
The present invention relates to a kind of organo-mineral complexing nanometer microwave absorbing material, it is composited by Kynoar with nanomorphic inorganic material；Wherein described inorganic material includes metal, metal oxide, metal sulfide or composite oxide of metal.The invention further relates to the preparation method of the organo-mineral complexing nanometer microwave absorbing material, it comprises the following steps：(1) Kynoar and nanomorphic inorganic material are dissolved in organic solvent, stirring obtains mixture；(2) solvent in said mixture is evaporated complete, obtains the organo-mineral complexing nanometer microwave absorbing material.The organo-mineral complexing nanometer microwave absorbing material of the present invention is prepared using solvent blending method, and preparation method is simple and can be directly prepared into film-form；Obtained microwave absorbing material stable homogeneous, while having certain pliability.
Description
Technical field
The invention belongs to microwave absorbing material technical field, and in particular to a kind of having with good microwave absorption capacity
Machine-inorganic composite nano microwave absorbing material and preparation method thereof.
Background technology
Microwave absorbing material, as the basic material of contemporary aircraft, weaponry etc., is the important of Modern Stealth Technique
Support, the focus that just always the military of various countries develops after World War II.In recent years, as various radio communications are set
The electronic technology such as standby, computer, remote sensing are developed rapidly, and the hazards of electromagnetic radiation that electronic product is brought is so that microwave absorption
Material is received much attention.Therefore, to the research of microwave absorbing material either at military aspect or civilian aspect
It is all significant.
Traditional research to microwave absorbing material is mainly based on nanomorphic inorganic material and paraffin to be combined, due to
Paraffin is softer in itself and fusing point is low, causes the stability of such microwave absorbing material poor, and its application is very limited.And this
Invention is combined as microwave absorbing material from Kynoar (PVDF) and nanomorphic inorganic material and carries out inhaling ripple research.It is poly-
Vinylidene (PVDF) is a kind of typical dielectric material, and it has good film forming and tailorability.In addition, PVDF
Also there is excellent wearability, pliability and impact resistance intensity.Most importantly, PVDF and the nanometer of nanomorphic inorganic material
The interfacial effect of structure and cooperative effect therebetween, have obvious enhancing to make the absorbing property of microwave absorbing material
With considerably increasing the practicality of microwave absorbing material.
The content of the invention
It is an object of the invention to provide a kind of Organic-inorganic composite nanometer microwave suction with good microwave absorption capacity
Material is received, film-form and stable homogeneous can be made in it, while having certain pliability.The present invention also aims to
Simple solvent blending method prepares the Organic-inorganic composite nanometer microwave absorbing material.
First aspect present invention is related to a kind of Organic-inorganic composite nanometer microwave absorbing material, its by Kynoar with
Nanomorphic inorganic material is composited；It is multiple that wherein described inorganic material includes metal, metal oxide, metal sulfide or metal
Close oxide.Wherein described nanomorphic inorganic material can be obtained using any preparation method existing in the prior art, for example
Hydro-thermal method.
In a preferred embodiment of the present invention, the metal is Co；The metal oxide is Co3O4；The metal sulphur
Compound is MoS2Or CuS；The composite oxide of metal is MnFe2O4。
Second aspect of the present invention is related to the Organic-inorganic composite nanometer microwave absorbing material described in first aspect present invention
Preparation method, it comprises the following steps：
(1) Kynoar and nanomorphic inorganic material are dissolved in organic solvent, stirring obtains mixture；
(2) solvent in said mixture is evaporated complete, obtains the Organic-inorganic composite nanometer microwave and absorb material
Material.Preferably, the solvent evaporation in the mixture can be carried out at high temperature, for example can be by the mixture at 100 DEG C
Baking oven in dry 1-3 hours.
In a preferred embodiment of the present invention, the organic solvent is DMF (DMF) or N, N- bis-
Methylacetamide (DMAc).
In a preferred embodiment of the present invention, the inorganic material is metal, metal oxide, metal sulfide or gold
Belong to composite oxides.
In a preferred embodiment of the present invention, the metal is Co；The metal oxide is Co3O4；The metal sulphur
Compound is MoS2Or CuS；The composite oxide of metal is MnFe2O4。
In a preferred embodiment of the present invention, the Kynoar and the mass ratio of the nanomorphic inorganic material are
20：1-1:1.
In a preferred embodiment of the present invention, the mass ratio of the Kynoar and the organic solvent is 1:50-
1:200。
In a preferred embodiment of the present invention, the mixture is placed in flat-shaped container and made in step (2)
Solvent evaporation obtains film-like microwave absorbing material completely, or absorbs material the Organic-inorganic composite nanometer microwave is made
Tabletting is carried out to it after material and obtains film-like microwave absorbing material.For example, the flat-shaped container can be culture dish or similar
The container of shape.
The advantage of the invention is that：The Organic-inorganic composite nanometer microwave absorbing material of the present invention is relative to prior art
It is middle that nanomorphic inorganic material and paraffin are combined for obtained microwave absorbing material, there is stable homogeneous, and this hair
Bright microwave absorbing material also has certain pliability, considerably increases the practicality of the microwave absorbing material of the present invention.This
The microwave absorbing material of invention uses solvent blending method, and reaction condition is gentle and preparation method is simple.Most of all, of the invention
Microwave absorbing material in PVDF and the nanostructured of nanomorphic inorganic material interfacial effect and therebetween cooperate with effect
Should, there is obvious humidification to the absorbing property of microwave absorbing material.
Brief description of the drawings
Reflection loss figures of the Fig. 1 for the microwave absorbing material in comparative example 1 of the present invention under each thickness.
Reflection loss figures of the Fig. 2 for the microwave absorbing material in comparative example 2 of the present invention under each thickness.
Fig. 3 is PVDF-MoS in the embodiment of the present invention 12Reflection loss of the nano combined microwave absorbing material under each thickness
Figure.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.It should be appreciated that described herein
Specific embodiment is only to explain technical key point, and protection scope of the present invention should include all interior of claim
Hold, but not limited to this.
Comparative example 1
By nanomorphic MoS2With paraffin according to mass ratio 1:1 compound obtained microwave absorbing material A.
Wherein described nanomorphic MoS2Prepared by hydro-thermal method, its preparation method comprises the following steps：By 0.1g
Na2MoO4·2H2O and 0.2g Cys are dissolved in 50ml water, and mixture is put into closed reactor after stirring,
Then the closed reactor is put into baking oven, in reacting 12h under 200 DEG C of self-generated pressures；After temperature drops to room temperature, it will react
Mixture afterwards takes out, and with deionized water and ethanol cleaning sample several times, sample finally is placed in into 60 DEG C of baking ovens, dries, treats
With.
Comparative example 2
Microwave absorbing material B is used as using pure Kynoar (PVDF).
Embodiment 1
Organic-inorganic composite nanometer microwave absorbing material C is prepared in accordance with the following steps：
1g Kynoar (PVDF) is dissolved in 100g organic solvents DMF (DMF), under normal temperature
It is continuously agitated；After after solution clear, 0.25g nanomorphics MoS is added thereto2, continue to stir a period of time；Finally,
Above-mentioned solution is all poured into culture dish, is placed in drying 2 hours in 100 DEG C of baking oven, is taken out after after solvent evaporation completely
Obtain the PVDF-MoS2Composite Nano microwave absorbing material (wherein, the "-" represent organic matter before and after it with it is inorganic
The compound implication of thing).
Wherein described nanomorphic MoS2Prepared by hydro-thermal method, its preparation method comprises the following steps：By 0.1g
Na2MoO4·2H2O and 0.2g Cys are dissolved in 50ml water, and mixture is put into closed reactor after stirring,
Then the closed reactor is put into baking oven, in reacting 12h under 200 DEG C of self-generated pressures；After temperature drops to room temperature, it will react
Mixture afterwards takes out, and with deionized water and ethanol cleaning sample several times, sample finally is placed in into 60 DEG C of baking ovens, dries, treats
With.
Above-mentioned microwave absorbing material A, B, C are subjected to tabletting successively, tabletting method is as follows：Each material is respectively put into mould
Afterwards, first each material is heated, (for microwave absorbing material C, PVDF melts under this state after temperature is raised to 210 DEG C
Change, and nanomorphic MoS2Do not melt), maintain a period of time；Then begin to pressurization, and pressurize 10 minutes；Finally stop heating, treat it
Drop to after room temperature, take out tabletting, it is to be measured.Tabletting is carried out using specific mould, above-mentioned microwave absorbing material A, B, C are pressed successively
Into external diameter be 7mm, internal diameter 3.04mm, thickness be 2mm, 2.5mm, 3mm, 3.5mm, 4mm, 4.5mm and 5mm sequin, then
Corresponding ripple of inhaling is carried out using Network Analyzer to test.Described microwave absorbing material A, B, C test result difference are as shown in Figure 1, Figure 2
With shown in Fig. 3.
With simple MoS it can be seen from Fig. 1, Fig. 2 and Fig. 32Or simple PVDF absorbing property is compared, PVDF-MoS2It is multiple
The absorbing property of nanometer microwave absorbing material is closed not between simple MoS2Certain value between simple PVDF, but compare the two and inhale
The superposition of ripple performance is also superior, has in the microwave absorbing material of this explanation present invention between PVDF and nanomorphic inorganic material
Certain cooperative effect, thus have obvious humidification to the absorbing property of microwave absorbing material.In MoS2Content is 20wt%
PVDF-MoS2In composite Nano microwave absorbing material, its minimum reflection loss value can reach -19.6dB under 5.0mm thickness
(6.0GHz), equivalent to about 99% electromagnetism wave energy is absorbed, and with the change of thickness, reflection loss value is less than -10dB
Frequency range be 5.04-15.36GHz.
Claims (7)
1. a kind of Organic-inorganic composite nanometer microwave absorbing material, it is characterised in that it is inorganic with nanomorphic by Kynoar
Material cladding is formed；Wherein described inorganic material is MoS2。
2. the preparation method of Organic-inorganic composite nanometer microwave absorbing material according to claim 1, it is characterised in that
It comprises the following steps：
(1) Kynoar and nanomorphic inorganic material are dissolved in organic solvent, stirring obtains mixture；
(2) solvent in said mixture is evaporated complete, obtains the Organic-inorganic composite nanometer microwave absorbing material.
3. preparation method according to claim 2, it is characterised in that the organic solvent be DMF or
DMAC N,N' dimethyl acetamide.
4. preparation method according to claim 2, it is characterised in that the inorganic material is MoS2。
5. preparation method according to claim 2, it is characterised in that the Kynoar and the inorganic material of the nanomorphic
The mass ratio of material is 20：1-1:1.
6. preparation method according to claim 2, it is characterised in that the matter of the Kynoar and the organic solvent
Amount is than being 1:50-1:200.
7. preparation method according to claim 2, it is characterised in that the mixture is placed in flat board in step (2)
In shape container and solvent evaporation is obtained film-like microwave absorbing material completely, or received in the obtained Organic-inorganic composite
Tabletting is carried out to it after rice microwave absorbing material and obtains film-like microwave absorbing material.
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| CN105883921A (en) * | 2016-04-14 | 2016-08-24 | 北京航空航天大学 | Preparation of 3D molybdenum disulfide nano-microparticles with high broadband wave absorption capability |
| CN106398056B (en) * | 2016-09-05 | 2018-11-13 | 北京航空航天大学 | Involve the composite material and preparation method of capability of electromagnetic shielding with excellent suction |
| CN106675516B (en) * | 2016-11-30 | 2018-07-06 | 中国人民解放军国防科学技术大学 | A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent and preparation method thereof |
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| CN1781872A (en) * | 2005-10-28 | 2006-06-07 | 清华大学 | Composite material with capacitance and inductance performance and its preparing method |
| CN1867243A (en) * | 2006-05-23 | 2006-11-22 | 清华大学 | Novel electromagnetic shielding composite material and its preparing method |
| CN103951916A (en) * | 2014-04-29 | 2014-07-30 | 南昌航空大学 | RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof |
| CN104558978A (en) * | 2014-12-15 | 2015-04-29 | 东莞市长安东阳光铝业研发有限公司 | Fluorine-containing polymer-based dielectric composite film and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1781872A (en) * | 2005-10-28 | 2006-06-07 | 清华大学 | Composite material with capacitance and inductance performance and its preparing method |
| CN1867243A (en) * | 2006-05-23 | 2006-11-22 | 清华大学 | Novel electromagnetic shielding composite material and its preparing method |
| CN103951916A (en) * | 2014-04-29 | 2014-07-30 | 南昌航空大学 | RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof |
| CN104558978A (en) * | 2014-12-15 | 2015-04-29 | 东莞市长安东阳光铝业研发有限公司 | Fluorine-containing polymer-based dielectric composite film and preparation method thereof |
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