CN105062417A - Organic-inorganic composite nano microwave absorbing material and preparation method thereof - Google Patents
Organic-inorganic composite nano microwave absorbing material and preparation method thereof Download PDFInfo
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- CN105062417A CN105062417A CN201510416495.0A CN201510416495A CN105062417A CN 105062417 A CN105062417 A CN 105062417A CN 201510416495 A CN201510416495 A CN 201510416495A CN 105062417 A CN105062417 A CN 105062417A
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Abstract
The invention relates to an organic-inorganic composite nano microwave absorbing material. The organic-inorganic composite nano microwave absorbing material is prepared by compositing polyvinylidene fluoride and a nano-state inorganic composite material, wherein the inorganic material comprises metal, metal oxide, metal sulfide or metal composite oxide. The invention further relates to a preparation method for the organic-inorganic composite nano microwave absorbing material. The preparation method comprises the following steps: (1) dissolving polyvinylidene fluoride and the nano-state inorganic composite material in an organic solvent, and stirring to obtain a mixture; (2) evaporating the solvent in the mixture completely to obtain the organic-inorganic composite nano microwave absorbing material. The organic-inorganic composite nano microwave absorbing material is prepared through a solvent blending method, is simple in preparation method, can be directly manufactured into a thin film, is uniform and stable, and meanwhile, has a certain degree of flexibility.
Description
Technical field
The invention belongs to microwave absorbing material technical field, be specifically related to a kind of Organic-inorganic composite nanometer microwave absorbing material with good microwave absorption capacity and preparation method thereof.
Background technology
Microwave absorbing material, as the base mateiral of contemporary aircraft, weaponry etc., is the important support of Modern Stealth Technique, is just the focus of the military of various countries development after World War II always.In recent years, along with the develop rapidly of the electronic technology such as various Wireless Telecom Equipment, computer, remote sensing, the hazards of electromagnetic radiation that electronic product brings makes microwave absorbing material receive much attention.Therefore, to the research of microwave absorbing material be military aspect or civilian in all significant.
Traditional research to microwave absorbing material is mainly to be complex as master by nanomorphic inorganic materials and paraffin, and because paraffin itself is softer and fusing point is low, cause the poor stability of such microwave absorbing material, its applicability is very limited.And the present invention selects polyvinylidene difluoride (PVDF) (PVDF) and nanomorphic inorganic materials compound as microwave absorbing material and carries out the research of suction ripple.Polyvinylidene difluoride (PVDF) (PVDF) is a kind of typical dielectric materials, and it has good film-forming properties and tailorability.In addition, PVDF also has excellent wear resistance, snappiness and shock-resistance intensity.Most importantly, the interfacial effect of the nanostructure of PVDF and nanomorphic inorganic materials and synergistic effect therebetween, have obvious enhancement to the absorbing property of microwave absorbing material, considerably increase the practicality of microwave absorbing material.
Summary of the invention
The object of the present invention is to provide a kind of Organic-inorganic composite nanometer microwave absorbing material with good microwave absorption capacity, it can make film like and stable homogeneous, has certain snappiness simultaneously.The present invention also aims to prepare this Organic-inorganic composite nanometer microwave absorbing material with simple solvent blending method.
First aspect present invention relates to a kind of Organic-inorganic composite nanometer microwave absorbing material, and it is composited by polyvinylidene difluoride (PVDF) and nanomorphic inorganic materials; Wherein said inorganic materials comprises metal, metal oxide, metallic sulfide or composite oxide of metal.Wherein said nanomorphic inorganic materials can adopt existing preparation method in any prior art to obtain, such as hydrothermal method.
In a preferred embodiment of the present invention, described metal is Co; Described metal oxide is Co
3o
4; Described metallic sulfide is MoS
2or CuS; Described composite oxide of metal is MnFe
2o
4.
Second aspect present invention relates to the preparation method of the Organic-inorganic composite nanometer microwave absorbing material described in first aspect present invention, and it comprises the following steps:
(1) polyvinylidene difluoride (PVDF) and nanomorphic inorganic materials are dissolved in organic solvent, stir and obtain mixture;
(2) by the solvent evaporation in said mixture completely, described Organic-inorganic composite nanometer microwave absorbing material is obtained.Preferably, the solvent evaporation in described mixture can at high temperature be carried out, such as can by described mixture dry 1-3 hour in the baking oven of 100 DEG C.
In a preferred embodiment of the present invention, described organic solvent is DMF (DMF) or N,N-dimethylacetamide (DMAc).
In a preferred embodiment of the present invention, described inorganic materials is metal, metal oxide, metallic sulfide or composite oxide of metal.
In a preferred embodiment of the present invention, described metal is Co; Described metal oxide is Co
3o
4; Described metallic sulfide is MoS
2or CuS; Described composite oxide of metal is MnFe
2o
4.
In a preferred embodiment of the present invention, the mass ratio of described polyvinylidene difluoride (PVDF) and described nanomorphic inorganic materials is 20:1-1:1.
In a preferred embodiment of the present invention, the mass ratio of described polyvinylidene difluoride (PVDF) and described organic solvent is 1:50-1:200.
In a preferred embodiment of the present invention, in step (2), described mixture is placed in flat-shaped container and solvent is evaporated and obtain film-like microwave absorbing material completely, or after obtained described Organic-inorganic composite nanometer microwave absorbing material, compressing tablet is carried out to it and obtain film-like microwave absorbing material.Such as, described flat-shaped container can be the container of culture dish or analogous shape.
The invention has the advantages that: Organic-inorganic composite nanometer microwave absorbing material of the present invention is for microwave absorbing material nanomorphic inorganic materials and paraffin compound obtained in prior art, there is the advantage of stable homogeneous, and microwave absorbing material of the present invention also has certain snappiness, considerably increase the practicality of microwave absorbing material of the present invention.Microwave absorbing material of the present invention adopts solvent blending method, and reaction conditions is gentle and preparation method is simple.The most important thing is, in microwave absorbing material of the present invention, the interfacial effect of the nanostructure of PVDF and nanomorphic inorganic materials and synergistic effect therebetween, have obvious enhancement to the absorbing property of microwave absorbing material.
Accompanying drawing explanation
Fig. 1 is the reflection loss figure of microwave absorbing material under each thickness in comparative example 1 of the present invention.
Fig. 2 is the reflection loss figure of microwave absorbing material under each thickness in comparative example 2 of the present invention.
Fig. 3 is PVDF-MoS in the embodiment of the present invention 1
2the reflection loss figure of nano combined microwave absorbing material under each thickness.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only in order to explain technical essential of the present invention, protection scope of the present invention should comprise the full content of claim, but is not limited thereto.
Comparative example 1
By nanomorphic MoS
2microwave absorbing material A is obtained according to mass ratio 1:1 compound with paraffin.
Wherein said nanomorphic MoS
2prepared by hydrothermal method, its preparation method comprises the following steps: by 0.1gNa
2moO
42H
2o and 0.2gL-halfcystine is dissolved in 50ml water, after stirring, mixture is put into closed reactor, subsequently this closed reactor is put into baking oven, under 200 DEG C of autogenous pressures, react 12h; Drop to after room temperature until temperature, reacted mixture is taken out, and with deionized water and ethanol purge sample number time, finally sample is placed in 60 DEG C of baking ovens, dry, stand-by.
Comparative example 2
Using pure polyvinylidene difluoride (PVDF) (PVDF) as microwave absorbing material B.
Embodiment 1
Prepare Organic-inorganic composite nanometer microwave absorbing material C in accordance with the following steps:
1g polyvinylidene difluoride (PVDF) (PVDF) is dissolved in 100g organic solvent DMF (DMF), ceaselessly stirs under normal temperature; After solution clear, add 0.25g nanomorphic MoS wherein
2, continue to stir for some time; Finally, above-mentioned solution is all poured in culture dish, and dry 2 hours of the baking oven being placed in 100 DEG C, take out after solvent evaporation completely and namely obtain described PVDF-MoS
2composite Nano microwave absorbing material (wherein, described "-" represents the implication of organism before and after it and inorganics compound).
Wherein said nanomorphic MoS
2prepared by hydrothermal method, its preparation method comprises the following steps: by 0.1gNa
2moO
42H
2o and 0.2gL-halfcystine is dissolved in 50ml water, after stirring, mixture is put into closed reactor, subsequently this closed reactor is put into baking oven, under 200 DEG C of autogenous pressures, react 12h; Drop to after room temperature until temperature, reacted mixture is taken out, and with deionized water and ethanol purge sample number time, finally sample is placed in 60 DEG C of baking ovens, dry, stand-by.
Above-mentioned microwave absorbing material A, B, C are carried out compressing tablet successively, tabletting method is as follows: after each material is put into mould respectively, first heat each material, after temperature is raised to 210 DEG C (for microwave absorbing material C, PVDF fusing under this state, and nanomorphic MoS
2do not melt), maintain for some time; Start pressurization subsequently, and pressurize 10 minutes; Finally stop heating, drop to after room temperature until it, take out compressing tablet, to be measured.Specific mould is adopted to carry out compressing tablet, above-mentioned microwave absorbing material A, B, C are pressed into successively external diameter is 7mm, internal diameter 3.04mm, thickness are the sequin of 2mm, 2.5mm, 3mm, 3.5mm, 4mm, 4.5mm and 5mm, adopt network analyzer to inhale ripple test accordingly subsequently.The test result of described microwave absorbing material A, B, C respectively as shown in Figure 1, Figure 2 and Figure 3.
As can be seen from Fig. 1, Fig. 2 and Fig. 3, with simple MoS
2or the absorbing property of simple PVDF is compared, PVDF-MoS
2the absorbing property of composite Nano microwave absorbing material is not between simple MoS
2and certain value between simple PVDF, but it is also more superior than the superposition of the two absorbing property, this illustrates in microwave absorbing material of the present invention to have certain synergistic effect between PVDF and nanomorphic inorganic materials, thus has obvious enhancement to the absorbing property of microwave absorbing material.At MoS
2content is the PVDF-MoS of 20wt%
2in composite Nano microwave absorbing material, its minimum reflection loss value can reach-19.6dB (6.0GHz) under 5.0mm thickness, the electromagnetism wave energy being equivalent to about 99% is absorbed, and along with the change of thickness, reflection loss value is 5.04-15.36GHz lower than the range of frequency of-10dB.
Claims (9)
1. an Organic-inorganic composite nanometer microwave absorbing material, is characterized in that, it is composited by polyvinylidene difluoride (PVDF) and nanomorphic inorganic materials; Wherein said inorganic materials comprises metal, metal oxide, metallic sulfide or composite oxide of metal.
2. Organic-inorganic composite nanometer microwave absorbing material according to claim 1, is characterized in that, described metal is Co; Described metal oxide is Co
3o
4; Described metallic sulfide is MoS
2or CuS; Described composite oxide of metal is MnFe
2o
4.
3. the preparation method of Organic-inorganic composite nanometer microwave absorbing material according to claim 1, it is characterized in that, it comprises the following steps:
(1) polyvinylidene difluoride (PVDF) and nanomorphic inorganic materials are dissolved in organic solvent, stir and obtain mixture;
(2) by the solvent evaporation in said mixture completely, described Organic-inorganic composite nanometer microwave absorbing material is obtained.
4. preparation method according to claim 3, is characterized in that, described organic solvent is DMF or N,N-dimethylacetamide.
5. preparation method according to claim 3, is characterized in that, described inorganic materials is metal, metal oxide, metallic sulfide or composite oxide of metal.
6. preparation method according to claim 5, is characterized in that, described metal is Co; Described metal oxide is Co
3o
4; Described metallic sulfide is MoS
2or CuS; Described composite oxide of metal is MnFe
2o
4.
7. preparation method according to claim 3, is characterized in that, the mass ratio of described polyvinylidene difluoride (PVDF) and described nanomorphic inorganic materials is 20:1-1:1.
8. preparation method according to claim 3, is characterized in that, the mass ratio of described polyvinylidene difluoride (PVDF) and described organic solvent is 1:50-1:200.
9. preparation method according to claim 3, it is characterized in that, in step (2), described mixture is placed in flat-shaped container and solvent is evaporated and obtain film-like microwave absorbing material completely, or after obtained described Organic-inorganic composite nanometer microwave absorbing material, compressing tablet is carried out to it and obtain film-like microwave absorbing material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106398056A (en) * | 2016-09-05 | 2017-02-15 | 北京航空航天大学 | Composite material with excellent wave absorption and electromagnetic shielding performances and preparation method thereof |
| CN106675516A (en) * | 2016-11-30 | 2017-05-17 | 中国人民解放军国防科学技术大学 | Transition metal chalcogenide-carbonyl iron powder 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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2015
- 2015-07-15 CN CN201510416495.0A patent/CN105062417B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106398056A (en) * | 2016-09-05 | 2017-02-15 | 北京航空航天大学 | Composite material with excellent wave absorption and electromagnetic shielding performances and preparation method thereof |
| CN106675516A (en) * | 2016-11-30 | 2017-05-17 | 中国人民解放军国防科学技术大学 | Transition metal chalcogenide-carbonyl iron powder composite microwave absorbent and preparation method thereof |
| 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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| CN105062417B (en) | 2017-07-21 |
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Effective date of registration: 20190724 Address after: 100070 Room 601, Building 3, 128 South Fourth Ring West Road, Fengtai District, Beijing Patentee after: PAYONEL ENVIRONMENTAL PURIFICATION ENGINEERING (BEIJING) CO., LTD. Address before: 100070 Beijing Fengtai District South Fourth Ring West Road 128 Courtyard 3, 5th floor 601-2 (Park) Patentee before: BEIJING XINYIYUAN ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD. |
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