CN107603087A - Composite wave-absorbing material and preparation method thereof - Google Patents
Composite wave-absorbing material and preparation method thereof Download PDFInfo
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- CN107603087A CN107603087A CN201710982168.0A CN201710982168A CN107603087A CN 107603087 A CN107603087 A CN 107603087A CN 201710982168 A CN201710982168 A CN 201710982168A CN 107603087 A CN107603087 A CN 107603087A
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- rgo
- iron oxide
- shell structure
- kynoar
- oxide core
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Abstract
The invention discloses an RGO/iron oxide filled polyvinylidene fluoride composite wave-absorbing material and a preparation method thereof, wherein the composite wave-absorbing material comprises RGO/iron oxide core-shell structure nano particles and polyvinylidene fluoride; the mass ratio of RGO to iron oxide in the RGO/iron oxide core-shell structure nano particles is 20 percent to 80 percent, the mass ratio of RGO/iron oxide core-shell structure nano particles in the composite wave-absorbing material is 1-20 percent, and the mass ratio of polyvinylidene fluoride is 80-99 percent.
Description
Technical field
The present invention relates to inorganic/organic composite absorbing material and preparation method thereof, and in particular to a kind of RGO/ iron oxide is filled out
Kynoar composite wave-suction material filled and preparation method thereof.
Technical background
The research and application of material obsorbing radar waves (abbreviation absorbing material) are the key factors of stealth technology development.With
The continuous development of the radar exploration technique, huge challenge is proposed to absorbing material, there is an urgent need to collect " thickness of thin, light weight, frequency
Duan Kuan, absorb it is strong " the advantages that the whole body multifunctional ceiling wave material.Traditional absorbing material often exist frequency band is narrow, density is big,
With thickness it is big the shortcomings of, it is difficult to meet above-mentioned composite request.
Graphene (graphene) be grow up recent years it is a kind of by carbon atom with sp2 hydridization bonding form two
Tie up periodic cellular shape lattice structure carbon material.Graphene has substantial amounts of electron channel, and effectively microwave energy can be changed into
Heat energy, it is a kind of potential lightweight microwave absorbing material [X.Sun, J.He, G.Li, J.Tang, T.Wang, Y.Guo and
H.Xue, Journal of Materials Che mistry C 2013,1,765-777.].It is raw material using graphite, leads to
Cross chemistry redox method, can prepare on a large scale graphene-based nanometer sheet RGO (also known as：The graphene oxide of reduction).It is based on
The oxy radical and defect of its remained on surface and suitable electric conductivity, the graphite that compares, CNT and high quality graphite
Alkene, RGO show more excellent microwave absorbing property [C.Wang, X.Han, P.Xu, X.Zhang, Y.Du, S.Hu, J.Wang and
X.Wang, Applied Ph ysics Letters 2011,98,072906.].However, due to the stronger Van der Waals of piece interlayer
Power, RGO easily assemble, and have a strong impact on its performance.
The content of the invention
It is an object of the invention to solve the problems, such as that prior art is present, there is provided a kind of poly- inclined fluorine of RGO/ iron oxide filling
Ethene composite wave-suction material, the material have the characteristics of good light weight, corrosion-resistant, absorbing property and easy processing；Preparation method
Simply, it is adapted to industrialized production.
The technical scheme is that：A kind of Kynoar of RGO/ iron oxide core-shell structure nanometer particle filling is compound
Absorbing material, the material include：RGO/ iron oxide core-shell structure nanometer particle is as inorganic non-metallic filler, Kynoar
For polymeric matrix；It is characterized in that mass ratio shared by each composition is：RGO/ iron oxide core-shell structure nanometer particle 1-20%, gather
Vinylidene 80-99%；Iron oxide is to be wrapped in form core shell structure by RGO in described RGO/ ferric oxide nano particles；RGO
Thickness be 0.37nm-5nm, structure is single or multiple lift；The particle diameter of iron oxide is 120nm-200nm, is shaped as polyhedron, knot
Structure is monocrystalline.
RGO/ iron oxide core-shell structure nanometer particle of the present invention, including：RGO nanoscale twins and iron oxide, its quality
Than for 20%：80%.
Currently preferred composition is RGO/ iron oxide core-shell structure nanometer particle 5%, Kynoar 95%；The composition
When, maximum reflection of the composite wave-suction material when thickness is 2mm is lost is issued to -39.43dB in frequency 14Hz, and reflection loss is low
Reach 6.0GHz (11.28~17.28GHz) in -10dB bandwidth.
RGO/ iron oxide core-shell structure nanometer particles used in the present invention are prepared by simple wet chemical method, gather inclined fluorine
Ethene is industrial products, and without any processing, so prepared by this composite, simple, cost is cheap, is adapted to industrialized production.
The tool of the Kynoar composite wave-suction material of RGO/ iron oxide core-shell structure nanometer particle filling of the present invention
Preparation：
Step 1：RGO/ iron oxide core-shell structure nanometer particles；In 2L three-neck flasks under strong stirring, successively will
0.555g polypyrroles alkanone and 4mL 80wt% hydrazine hydrate solutions are added in 1.5L 0.25mg/mL graphene oxide solutions,
It is heated to adding after 90 DEG C and isothermal reaction 2 hours 30mL 2.5M ferric chloride solutions under stirring condition, then heats to 100 DEG C
Isothermal reaction 24 hours, is then cooled to room temperature, is isolated by filtration, and 60 DEG C of dryings 24 after fully being washed with deionized water
Hour, collect black product；
Step 2：Weigh in mass ratio 1-20% RGO/ iron oxide core-shell structure nanometer particle and 80-99% it is poly- partially
PVF (each component sum is 100%), adds DMF, sonic oscillation 1h, makes RGO/ iron oxide core shell structures
Naturally dry after nano-particle and Kynoar are well mixed；
Step 3：Compound obtained by step 2 is fitted into mould, on hot press, 180-200 DEG C, under 10-20MPa
30min, then pressurize cooling are molded, that is, prepares the compound suction of Kynoar of RGO/ iron oxide core-shell structure nanometer particle filling
Wave material；
The advantage of the invention is that：(1) composite prepared by the present invention has unique structure and physicochemical property,
Such as：Inorganic/inorganic interface possessed by the unique core shell structure of inorganic non-metallic filler RGO/ iron oxide and RGO/ are poly- inclined
What inorganic/organic interface structure between PVF, RGO excellent thermal conductivity and electrical conductance and RGO/ iron oxide surfaces were enriched
Oxy radical and unsaturated dangling bond are advantageous to the absorption and decay of electromagnetic wave；(2) composite is to 2-18GHz electromagnetism
Ripple has strong and wide electromagnetic absorption effect；(3) the composite light weight；(4) polymer matrix body phase contains in the composite
Amount is high, and the processing characteristics of composite is good, can be prepared into required shape.
Brief description of the drawings
Fig. 1 is RGO/ iron oxide core shell structure SEM photograph figures in the present invention.
Fig. 2 is the SEM photograph figure of composite section in the embodiment of the present invention 3.
Fig. 3 is reflection of electromagnetic wave attenuation curve of the composite when thickness is 2.0mm in embodiment 3 at room temperature.
Embodiment
Embodiment 1：Prepare the composite that RGO/ iron oxide core-shell structure nanometer particles mass ratio is 1wt%, specific step
It is rapid as follows：
(1)：Prepare RGO/ iron oxide core-shell structure nanometer particles；
(2)：1% RGO/ iron oxide core-shell structure nanometer particle and 99% Kynoar is weighed in mass ratio, is added
Enter DMF, sonic oscillation 1h, RGO/ iron oxide core-shell structure nanometer particle and Kynoar is mixed
It is even；
(3)：Compound obtained as above is fitted into mould, on hot press, 180 DEG C, be molded 30min under 15MPa, then
Pressurize cools down, that is, the Kynoar for preparing mass fraction as the filling of 1%RGO/ iron oxide core-shell structure nanometer particle is compound
Absorbing material.
Embodiment 2：Prepare Fe2O3Nano-particle mass ratio is 2% composite, is comprised the following steps that：
(1)：Prepare RGO/ iron oxide core-shell structure nanometer particles；
(2)：2% RGO/ iron oxide core-shell structure nanometer particle and 98% Kynoar is weighed in mass ratio, is added
Enter DMF, sonic oscillation 1h, RGO/ iron oxide core-shell structure nanometer particle and Kynoar is mixed
It is even；
(3)：Compound obtained as above is fitted into mould, on hot press, 180 DEG C, be molded 30min under 15MPa, then
Pressurize cools down, that is, the Kynoar for preparing mass fraction as the filling of 2%RGO/ iron oxide core-shell structure nanometer particle is compound
Absorbing material.
Embodiment 3：Prepare the composite that RGO/ iron oxide core-shell structure nanometer particles mass ratio is 5%, specific steps
It is as follows：
(1)：Prepare RGO/ iron oxide core-shell structure nanometer particles；
(2)：5% RGO/ iron oxide core-shell structure nanometer particle and 95% Kynoar is weighed in mass ratio, is added
Enter DMF, sonic oscillation 1h, RGO/ iron oxide core-shell structure nanometer particle and Kynoar is mixed
It is even；
(3)：Compound obtained as above is fitted into mould, on hot press, 180 DEG C, be molded 30min under 15MPa, then
Pressurize cools down, that is, the Kynoar for preparing mass fraction as the filling of 5%RGO/ iron oxide core-shell structure nanometer particle is compound
Absorbing material.
Embodiment 4：Prepare the composite that RGO/ iron oxide core-shell structure nanometer particles mass ratio is 10%, specific steps
It is as follows：
(1)：Prepare RGO/ iron oxide core-shell structure nanometer particles；；
(2)：10% RGO/ iron oxide core-shell structure nanometer particle and 90% Kynoar is weighed in mass ratio, is added
Enter DMF, sonic oscillation 1h, RGO/ iron oxide core-shell structure nanometer particle and Kynoar is mixed
It is even；
(3)：Compound obtained as above is fitted into mould, on hot press, 180 DEG C, be molded 30min under 15MPa, then
Pressurize cools down, that is, the Kynoar for preparing mass fraction as the filling of 10%RGO/ iron oxide core-shell structure nanometer particle is compound
Absorbing material.
Embodiment 5：Prepare the composite that RGO/ iron oxide core-shell structure nanometer particles mass ratio is 15%, specific steps
It is as follows：
(1)：Prepare RGO/ iron oxide core-shell structure nanometer particles；
(2)：15% RGO/ iron oxide core-shell structure nanometer particle and 85% Kynoar is weighed in mass ratio, is added
Enter DMF, sonic oscillation 1h, RGO/ iron oxide core-shell structure nanometer particle and Kynoar is mixed
It is even；
(3)：Compound obtained as above is fitted into mould, on hot press, 180 DEG C, be molded 30min under 15MPa, then
Pressurize cools down, that is, the Kynoar for preparing mass fraction as the filling of 15%RGO/ iron oxide core-shell structure nanometer particle is compound
Absorbing material.
Embodiment 6：Prepare the composite that RGO/ iron oxide core-shell structure nanometer particles mass ratio is 20%, specific steps
It is as follows：
(1)：Prepare RGO/ iron oxide core-shell structure nanometer particles
(2)：20% RGO/ iron oxide core-shell structure nanometer particle and 80% Kynoar is weighed in mass ratio, is added
Enter DMF, sonic oscillation 1h, RGO/ iron oxide core-shell structure nanometer particle and Kynoar is mixed
It is even；
(3)：Compound obtained as above is fitted into mould, on hot press, 180 DEG C, be molded 30min under 15MPa, then
Pressurize cools down, that is, the Kynoar for preparing mass fraction as the filling of 20%RGO/ iron oxide core-shell structure nanometer particle is compound
Absorbing material.
Claims (4)
1. a kind of Kynoar composite wave-suction material of RGO/ iron oxide filling, it includes：RGO/ iron oxide core shell structures are received
Rice corpuscles is polymeric matrix as inorganic non-metallic filler, Kynoar；It is characterized in that：Mass ratio shared by each composition
For：RGO/ iron oxide core-shell structure nanometer particle 1-20%, Kynoar 80-99%；Described RGO/ iron oxide nano-granules
Iron oxide is to be wrapped in form core shell structure by RGO in son；RGO thickness is 0.37nm-5nm, and structure is single or multiple lift；Oxygen
The particle diameter for changing iron is 120nm-200nm, is shaped as polyhedron, structure is monocrystalline.
2. a kind of Kynoar composite wave-suction material of RGO/ iron oxide filling according to claim 1, its feature exist
In：The RGO/ iron oxide core-shell structure nanometer particle, including RGO nanoscale twins and iron oxide, its mass ratio are 20%:
80%.
3. a kind of preparation method of the Kynoar composite wave-suction material of the iron oxide of RGO/ according to claim 1 filling,
It is characterized in that method and step is as follows：
The preparation method of inorganic RGO/ iron oxide core-shell structure nanometer particle；
The above-mentioned inorganic nano-particle prepared is mixed with organic polymer Kynoar.
A kind of 4. preparation side of the Kynoar composite wave-suction material of RGO/ iron oxide filling according to claim 3
Method, it is characterised in that：Preparation method in the step (1) is：In 2L three-neck flasks under strong stirring, successively by 0.555g
Polypyrrole alkanone and 4mL 80% hydrazine hydrate solution are added in 1.5L 0.25mg/mL graphene oxide solutions, stirring condition
Under be heated to adding after 90 DEG C and isothermal reaction 2 hours 30mL 2.5M ferric chloride solutions, then heat to 100 DEG C of isothermal reactions
24 hours, room temperature is then cooled to, is isolated by filtration, and 60 DEG C of dryings 24 hours after fully being washed with deionized water, receive
Collect black product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342036A (en) * | 2018-03-26 | 2018-07-31 | 南昌航空大学 | A kind of magnetism Mxenes polymer composite wave-suction materials and preparation method thereof |
| CN108342036B (en) * | 2018-03-26 | 2020-05-15 | 南昌航空大学 | Magnetic Mxenes polymer composite wave-absorbing material and preparation method thereof |
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