CN103951916A - RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof - Google Patents
RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof Download PDFInfo
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- CN103951916A CN103951916A CN201410176439.XA CN201410176439A CN103951916A CN 103951916 A CN103951916 A CN 103951916A CN 201410176439 A CN201410176439 A CN 201410176439A CN 103951916 A CN103951916 A CN 103951916A
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Abstract
The invention discloses an RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and a preparation method thereof. The composite wave-absorbing material comprises the following compositions in percentage by mass: 1-20% of RGO/ferric oxide nano-particles with a core-shell structure, and 80-99% of polyvinylidene fluoride; and the mass ratio of RGO to ferric oxide in the RGO/ferric oxide nano-particles with the core-shell structure is 20%:80%. The RGO/ferric oxide nano-particles with the core-shell structure are filled into polyvinylidene, when the mass ratio of inorganic nanoparticles is 5% and the inorganic/organic composite wave-absorbing material is 2mm thick, the maximum reflection loss achieves -39.43dB under the frequency of 14Hz, and the bandwidth of the reflection loss below -10dB achieves 6.0GHz (11.28-17.28GHz). The advantages are that the composite wave-absorbing material has the characteristics of being light in mass, corrosion-resistant, good in wave-absorbing property, easy to process and the like, and the preparation method is simple and easily realizes the industrial production.
Description
Technical field
The present invention relates to inorganic/organic composite absorbing material and preparation method thereof, be specifically related to polyvinylidene difluoride (PVDF) composite wave-suction material of a kind of RGO/ ferric oxide filling and preparation method thereof.
Technical background
The research of material obsorbing radar waves (abbreviation absorbing material) and application are the key factors of stealthy technique development.Along with the development of the radar exploration technique, absorbing material has been proposed to huge challenge, in the urgent need to the multifunctional ceiling wave material of the advantage the whole bodys such as collection " thin thickness, quality is light, frequency range is wide, absorptions be strong ".Often there is the shortcomings such as frequency band is narrow, density is large, matching thickness is large in traditional absorbing material, is difficult to meet above-mentioned composite request.
Graphene (graphene) is the cellular lattice structure carbon material of a kind of two-dimensional and periodic being formed with sp2 hydridization bonding by carbon atom growing up recent years.Graphene has a large amount of electron channels, can effectively microwave energy be changed into heat energy, 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 Chemistry C 2013,1,765-777.].Utilize graphite for starting material, by chemistry redox method, can prepare on a large scale graphene-based nanometer sheet RGO(and have another name called: the graphene oxide of reduction).Oxy radical based on its remained on surface and defect and suitable electroconductibility, compare graphite, carbon nanotube and high-quality graphene, RGO shows more excellent microwave absorbing property [C. Wang, X. Han, P. Xu, X. Zhang, Y. Du, S. Hu, J. Wang and X. Wang, Applied Physics Letters 2011,98,072906.].Yet due to the stronger Van der Waals force of sheet interlayer, RGO easily assembles, and has a strong impact on its performance.
Summary of the invention
The object of the invention is to solve the problem that prior art exists, the polyvinylidene difluoride (PVDF) composite wave-suction material that provides a kind of RGO/ ferric oxide to fill, this material has the advantages that quality is light, corrosion-resistant, absorbing property is good and easily process; Preparation method is simple, is applicable to suitability for industrialized production.
Technical scheme of the present invention is: the polyvinylidene difluoride (PVDF) composite wave-suction material that a kind of RGO/ ferric oxide core-shell structure nanometer particle is filled, and this material comprises: RGO/ ferric oxide core-shell structure nanometer particle is polymeric matrix as inorganic non-metallic weighting agent, polyvinylidene difluoride (PVDF); It is characterized in that the shared mass ratio of each composition is: RGO/ ferric oxide core-shell structure nanometer particle 1-20 %, polyvinylidene difluoride (PVDF) 80-99 %; In described RGO/ ferric oxide nano particles, ferric oxide is wrapped in formation nucleocapsid structure by RGO; The thickness of RGO is 0.37 nm-5nm, and structure is single or multiple lift; The particle diameter of ferric oxide is 120 nm-200 nm, is shaped as polyhedron, and structure is monocrystalline.
RGO/ ferric oxide core-shell structure nanometer particle of the present invention, comprising: RGO nanoscale twins and ferric oxide, its mass ratio is 20% ﹕ 80%.
The present invention preferably consists of RGO/ ferric oxide core-shell structure nanometer particle 5 %, polyvinylidene difluoride (PVDF) 95 %; When this forms, the maximum reflection loss of composite wave-suction material when thickness is 2 mm is issued to-39.43 dB at frequency 14 Hz, and reflection loss reaches 6.0 GHz (11.28～17.28 GHz) lower than the bandwidth of-10 dB.
The present invention's RGO/ ferric oxide core-shell structure nanometer particle used is prepared by simple wet chemical method, and polyvinylidene difluoride (PVDF) is Industrial products, without any processing, so prepared by this matrix material simple, with low cost, is applicable to suitability for industrialized production.
The concrete preparation method of the polyvinylidene difluoride (PVDF) composite wave-suction material that RGO/ ferric oxide core-shell structure nanometer particle of the present invention is filled:
Step 1: RGO/ ferric oxide core-shell structure nanometer particle; In 2 L three-necked flasks under strong stirring, successively the 80 wt % hydrazine hydrate solutions of 0.555 g polypyrrole alkane ketone and 4 mL are joined in the 0.25 mg/ mL graphene oxide solution of 1.5 L, under agitation condition, be heated to 90 ℃ and isothermal reaction add 30 mL 2.5 M ferric chloride Solutions after 2 hours, then be warming up to 100 ℃ of isothermal reactions 24 hours, be cooled to subsequently room temperature, by filtering separation, and with deionized water fully wash latter 60 ℃ dry 24 hours, collect black product;
Step 2: take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 1-20 % and the polyvinylidene difluoride (PVDF) of 80-99 % (each component sum is 100%), add N, N dimethyl formamide, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF) and naturally dries afterwards;
Step 3: the compound of step 2 gained is packed in mould, on thermocompressor, mold pressing 30min under 180-200 ℃, 10-20MPa, then pressurize is cooling, prepares the polyvinylidene difluoride (PVDF) composite wave-suction material that RGO/ ferric oxide core-shell structure nanometer particle is filled;
The invention has the advantages that: the prepared matrix material of (1) the present invention has unique structure and physico-chemical property, as: between inorganic/inorganic interface that nucleocapsid structure had of inorganic non-metallic weighting agent RGO/ ferric oxide uniqueness and RGO/ polyvinylidene difluoride (PVDF) inorganic/thermal conductivity of organic interface structure, RGO excellence and electric conductivity and abundant oxy radical and the unsaturated outstanding key of RGO/ iron oxide surface be all conducive to electromagnetic absorption and decay; (2) this matrix material has strong and wide electromagnetic absorption effect to 2-18 GHz hertzian wave; (3) this matrix material quality is light; (4) in this matrix material, polymeric matrix phase content is high, and the good processability of matrix material can be prepared into needed shape.
Accompanying drawing explanation
Fig. 1 is RGO/ ferric oxide nucleocapsid structure SEM photo figure in the present invention.
Fig. 2 is the SEM photo figure of matrix material section in the embodiment of the present invention 3.
Fig. 3 is the reflection of electromagnetic wave extinction curve of matrix material when thickness is 2.0 mm in embodiment 3 under room temperature.
Embodiment
Embodiment 1: preparation RGO/ ferric oxide core-shell structure nanometer particle mass ratio is the matrix material of 1 wt %, and concrete steps are as follows:
(1): preparation RGO/ ferric oxide core-shell structure nanometer particle;
(2): take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 1 % and the polyvinylidene difluoride (PVDF) of 99 %, add DMF, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF);
(3): the compound of above gained is packed in mould, on thermocompressor, mold pressing 30min under 180 ℃, 15MPa, then pressurize is cooling, preparing massfraction is the polyvinylidene difluoride (PVDF) composite wave-suction material that 1 % RGO/ ferric oxide core-shell structure nanometer particle is filled.
Embodiment 2: preparation Fe
2o
3nanoparticle mass ratio is the matrix material of 2 %, and concrete steps are as follows:
(1): preparation RGO/ ferric oxide core-shell structure nanometer particle;
(2): take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 2 % and the polyvinylidene difluoride (PVDF) of 98 %, add DMF, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF);
(3): the compound of above gained is packed in mould, on thermocompressor, mold pressing 30min under 180 ℃, 15MPa, then pressurize is cooling, preparing massfraction is the polyvinylidene difluoride (PVDF) composite wave-suction material that 2 % RGO/ ferric oxide core-shell structure nanometer particles are filled.
Embodiment 3: preparation RGO/ ferric oxide core-shell structure nanometer particle mass ratio is the matrix material of 5 %, and concrete steps are as follows:
(1): preparation RGO/ ferric oxide core-shell structure nanometer particle;
(2): take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 5 % and the polyvinylidene difluoride (PVDF) of 95 %, add DMF, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF);
(3): the compound of above gained is packed in mould, on thermocompressor, mold pressing 30min under 180 ℃, 15MPa, then pressurize is cooling, preparing massfraction is the polyvinylidene difluoride (PVDF) composite wave-suction material that 5 % RGO/ ferric oxide core-shell structure nanometer particles are filled.
Embodiment 4: preparation RGO/ ferric oxide core-shell structure nanometer particle mass ratio is the matrix material of 10 %, and concrete steps are as follows:
(1): preparation RGO/ ferric oxide core-shell structure nanometer particle; ;
(2): take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 10 % and the polyvinylidene difluoride (PVDF) of 90 %, add DMF, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF);
(3): the compound of above gained is packed in mould, on thermocompressor, mold pressing 30min under 180 ℃, 15MPa, then pressurize is cooling, preparing massfraction is the polyvinylidene difluoride (PVDF) composite wave-suction material that 10 % RGO/ ferric oxide core-shell structure nanometer particles are filled.
Embodiment 5: preparation RGO/ ferric oxide core-shell structure nanometer particle mass ratio is the matrix material of 15 %, and concrete steps are as follows:
(1): preparation RGO/ ferric oxide core-shell structure nanometer particle;
(2): take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 15 % and the polyvinylidene difluoride (PVDF) of 85 %, add DMF, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF);
(3): the compound of above gained is packed in mould, on thermocompressor, mold pressing 30min under 180 ℃, 15MPa, then pressurize is cooling, preparing massfraction is the polyvinylidene difluoride (PVDF) composite wave-suction material that 15 % RGO/ ferric oxide core-shell structure nanometer particles are filled.
Embodiment 6: preparation RGO/ ferric oxide core-shell structure nanometer particle mass ratio is the matrix material of 20 %, and concrete steps are as follows:
(1): preparation RGO/ ferric oxide core-shell structure nanometer particle;
(2): take in mass ratio the RGO/ ferric oxide core-shell structure nanometer particle of 20 % and the polyvinylidene difluoride (PVDF) of 80 %, add DMF, sonic oscillation 1h, mixes RGO/ ferric oxide core-shell structure nanometer particle and polyvinylidene difluoride (PVDF);
(3): the compound of above gained is packed in mould, on thermocompressor, mold pressing 30min under 180 ℃, 15MPa, then pressurize is cooling, preparing massfraction is the polyvinylidene difluoride (PVDF) composite wave-suction material that 20 % RGO/ ferric oxide core-shell structure nanometer particles are filled.
Claims (4)
1. the polyvinylidene difluoride (PVDF) composite wave-suction material that RGO/ ferric oxide is filled, it comprises: RGO/ ferric oxide core-shell structure nanometer particle is polymeric matrix as inorganic non-metallic weighting agent, polyvinylidene difluoride (PVDF); It is characterized in that: the shared mass ratio of each composition is: RGO/ ferric oxide core-shell structure nanometer particle 1-20 %, polyvinylidene difluoride (PVDF) 80-99 %; In described RGO/ ferric oxide nano particles, ferric oxide is wrapped in formation nucleocapsid structure by RGO; The thickness of RGO is 0.37 nm-5nm, and structure is single or multiple lift; The particle diameter of ferric oxide is 120 nm-200 nm, is shaped as polyhedron, and structure is monocrystalline.
2. the polyvinylidene difluoride (PVDF) composite wave-suction material that a kind of RGO/ ferric oxide according to claim 1 is filled, is characterized in that: described RGO/ ferric oxide core-shell structure nanometer particle, comprise RGO nanoscale twins and ferric oxide, and its mass ratio is 20% ﹕ 80%.
3. a preparation method for the polyvinylidene difluoride (PVDF) composite wave-suction material that RGO/ ferric oxide is filled according to claim 1, is characterized in that method steps is as follows:
The preparation method of inorganic RGO/ ferric oxide core-shell structure nanometer particle;
The above-mentioned inorganic nano-particle preparing is mixed with organic polymer polyvinylidene difluoride (PVDF).
4. the preparation method of the polyvinylidene difluoride (PVDF) composite wave-suction material that a kind of RGO/ ferric oxide according to claim 3 is filled, it is characterized in that: the preparation method in described step (1) is: in 2 L three-necked flasks under strong stirring, successively the 80 % hydrazine hydrate solutions of 0.555 g polypyrrole alkane ketone and 4 mL are joined in the 0.25 mg/ mL graphene oxide solution of 1.5 L, under agitation condition, be heated to 90 ℃ and isothermal reaction add 30 mL 2.5 M ferric chloride Solutions after 2 hours, then be warming up to 100 ℃ of isothermal reactions 24 hours, be cooled to subsequently room temperature, pass through filtering separation, and with deionized water, fully wash latter 60 ℃ and be dried 24 hours, collect black product.
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| 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 |
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| CN110835447A (en) * | 2019-12-02 | 2020-02-25 | 西安交通大学 | Ku waveband composite wave-absorbing material and preparation method thereof |
| CN115093518A (en) * | 2022-07-19 | 2022-09-23 | 四川大学 | Wave absorber with core-shell structure and preparation method thereof |
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| CN107107052A (en) * | 2015-11-11 | 2017-08-29 | 沙特基础工业全球技术公司 | The multiple function stable nanometer tectosome of hydrotalcite shell containing nano-sized carbon and nanostructured or micrometer structure and through calcining |
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| 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 |
| CN110305429A (en) * | 2019-07-15 | 2019-10-08 | 北京化工大学 | A kind of flexibility absorbing material and preparation method thereof |
| CN110835447A (en) * | 2019-12-02 | 2020-02-25 | 西安交通大学 | Ku waveband composite wave-absorbing material and preparation method thereof |
| CN115093518A (en) * | 2022-07-19 | 2022-09-23 | 四川大学 | Wave absorber with core-shell structure and preparation method thereof |
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