CN106398056B - Involve the composite material and preparation method of capability of electromagnetic shielding with excellent suction - Google Patents
Involve the composite material and preparation method of capability of electromagnetic shielding with excellent suction Download PDFInfo
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- CN106398056B CN106398056B CN201610803874.XA CN201610803874A CN106398056B CN 106398056 B CN106398056 B CN 106398056B CN 201610803874 A CN201610803874 A CN 201610803874A CN 106398056 B CN106398056 B CN 106398056B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
Abstract
The invention discloses a kind of composite material and preparation methods involving capability of electromagnetic shielding with excellent suction, belong to nanocomposite and its preparing technical field.The composite material includes rGO@MoS2Particle and PVDF, the rGO@MoS2The mass fraction of particle in the composite is 2.5~30wt%.When the mass fraction is 5wt%, the composite material has absorbing property；When the mass fraction is 25wt%, the composite material has shielding properties.Composite material preparation process provided by the invention is simple, and molybdenum disulfide nano ball is stablized, and the success rate compound with graphene oxide is very high, is expected to mass production；Composite material provided by the invention simultaneously there is excellent suction to involve capability of electromagnetic shielding.
Description
Technical field
The invention belongs to nanocomposite and its preparing technical fields, and in particular to a kind of that there is excellent suction to involve electricity
The composite material and preparation method of magnetic shield performance.
Background technology
In recent years, with the fast development of electronic equipment, the carrier that electromagnetic wave is propagated as information is in military, boat
The fields extensive use such as empty space flight, civilian.However, electromagnetic wave but brings problems, such as electromagnetic interference, electromagnetic radiation,
These all bring huge challenge to the health of people.
Interface impedance and energy loss by radiation are two key factors for determining absorbing material.The performance of absorbing material is situated between
Electric value ε, magnetic permeability value μ and conductivity value δ influence, these parameters are the intuitive reflections of the structure and performance of wave absorbing agent.Scientific research work
Authors are by adjusting the conductivity of material, dielectric constant and magnetic permeability value in the hope of low interface impedance and high lossy microwave.Currently,
The absorbing property of the materials such as metal powder, ceramics, ferrite has been studied, but most is due to density
Greatly, unstable etc. and be unable to practical application.
Electromagnetic shielding is one of the effective means for inhibiting interference, realizing electromagnetic protection.When electromagnetic radiation is by air directive screen
When covering material, reflection, refraction effect are will produce on the surface of material, multiple reflections phenomenon can occur in material internal.Electromagnetic screen
It covers and the purpose for inhibiting radiation exactly is realized to the reflection of electromagnetic radiation and refraction effect using material.Shield effectiveness SE is to weigh
The factor of material capability of electromagnetic shielding, it includes the absorption efficiency SE of shielding materialA, shield surface reflection performance SERAnd screen
Cover the multiple reflections efficiency SE in internal portionM.Reflection is related with the impedance matching of air and material, and absorption may be considered electromagnetic wave
Energy attenuation in the material, multiple reflections represent the scattering effect caused by material internal inhomogeneities, mainly occur
In the material at internal large area interface, such as porous material, mesh material.
It is compared with traditional electromagnetic shielding material based on metal, graphene conductive high molecular material is due to light, anti-corruption
Erosion, the advantages that processing technology is simple, surface area is big, dielectric radio is high receive people's concern.However, the electric conductivity and electricity of pure graphene
Magnetic property cannot meet impedance matching due to Tai Gao, people by its with other materials are compound studies.Molybdenum disulfide
It is a kind of semi-conducting material, there is high electron mobility, in electro-catalysis, photocatalysis, battery, biology, sensing and electronic equipment
Equal fields are widely used.
Invention content
It is an object of the invention to overcome current material only to have single absorbing property or capability of electromagnetic shielding not
Foot provides a kind of composite material that can have excellent suction to involve capability of electromagnetic shielding simultaneously, i.e., described composite material tool
It is improved the purposes inhaled wave amount or widen frequency absorption section, it is also possible that it is to be reflected that most of electromagnetic wave, which is absorbed without,.
The composite material provided by the invention for involving capability of electromagnetic shielding with excellent suction, the composite material include
rGO@MoS2Particle and PVDF, the rGO@MoS2The mass fraction of particle in the composite is 2.5~30wt%.Work as institute
When the mass fraction stated is 5wt%, the composite material has absorbing property；When the mass fraction is 25wt%,
The composite material has shielding properties.
The preparation method of the composite material for involving capability of electromagnetic shielding with excellent suction, includes the following steps：
The first step, by graphene oxide GO and MoS2With mass ratio for 1:1~4:1, it is dissolved in deionized water, ultrasound 1~
2h makes the two be mixed into the first mixed liquor.
Preferably, GO and MoS2Mass ratio be 2:1.
First mixed liquor is placed in 85~95 DEG C of oil baths by second step, after 5~10min, addition hydrazine hydrate, reaction 2~
3h.Last 2~4h of ultrasound again.
Third walks, and the product after ultrasound is centrifuged, is washed successively with water and ethyl alcohol, dry, obtains finely dispersed rGO@
MoS2Particle.
PVDF (Kynoar) is dissolved in 30mL n,N-Dimethylformamide by the 4th step, and ultrasound is until obtain transparent
The second mixed liquor.
5th step, by rGO@MoS2Particle is dissolved in above-mentioned second mixed liquor, and mechanical agitation obtains black suspension.By institute
The black suspension stated is transferred in evaporating dish, is placed in 4h in 70~100 DEG C of baking oven, and rGO@MoS are made after evaporating solvent2/
PVDF composite materials.
The rGO@MoS2In/PVDF composite materials, rGO@MoS2The mass fraction of particle is 2.5~30wt%.Work as institute
When the mass fraction stated is 5wt%, the composite material has absorbing property；When the mass fraction is 25wt%,
The composite material has shielding properties.
Compared with existing absorbing material, composite material of the invention has following advantage：
(1) composite material preparation process provided by the invention is simple, and molybdenum disulfide only can equably be divided by ultrasound
It is dispersed in rGO without carrying out other processing.
(2) molybdenum disulfide nano ball needed for composite material provided by the invention is stablized, and compound with graphene oxide
Success rate it is very high, be expected to mass production.
(3) after absorbing material prepared by the present invention is mixed with PVDF, the suction wave amount of material is not only greatly improved, but also
Frequency absorption section is broadened, therefore improves the absorbing property of material.
(4) composite material provided by the invention simultaneously there is excellent suction to involve capability of electromagnetic shielding.
(5) the preparation process majority of composite material provided by the invention is physical method, easy to operate, takes few, energy consumption
It is few and environmentally protective to accomplish without using other chemical reagent.
Description of the drawings
Fig. 1 is the rGO@MoS prepared in the embodiment of the present invention 12Scanning electron microscope (SEM) picture of particle；
Fig. 2 is 5.0wt%rGO@MoS prepared by the present invention2Reflection loss curve graph under/PVDF 1~5mm thickness；
Fig. 3 A~3C are respectively 25.0wt%rGO@MoS prepared by the present invention2The SE of/PVDF composite materialsTotal、SEAWith
SERValue is with frequency variation relation curve.
Specific implementation mode
The present invention is described in detail with reference to the accompanying drawings and examples.
The present invention provides a kind of composite material and preparation method involving capability of electromagnetic shielding with excellent suction, described
Composite material include rGO@MoS2Particle and PVDF, the rGO@MoS2The mass fraction of particle in the composite is 2.5
~30wt%.When the mass fraction is 5wt%, the composite material has absorbing property；When the quality point
When number is 25wt%, the composite material has shielding properties.
The above-mentioned rGO@MoS for involving capability of electromagnetic shielding with excellent suction2The preparation method of/PVDF composite materials, packet
Include following steps：
The first step, by GO and MoS2With mass ratio for 1:1~4:1, it is dissolved in deionized water, 1~2h of ultrasound keeps the two mixed
It closes uniformly at the first mixed liquor.
First mixed liquor is placed in 85~95 DEG C of oil baths by second step, after 5~10min, addition hydrazine hydrate, reaction 2~
3h.Last 2~4h of ultrasound again.The amount that hydrazine hydrate is wherein added is the 0.05% of deionized water volume.
Third walks, and the product after ultrasound is centrifuged, is washed successively with water and ethyl alcohol, dry, obtains finely dispersed rGO@
MoS2Particle.
PVDF is dissolved in 30mLN by the 4th step, and in dinethylformamide, ultrasound is until obtain the second transparent mixed liquor.
5th step, by rGO@MoS2Particle is dissolved in above-mentioned second mixed liquor, and mechanical agitation obtains black suspension.By institute
The black suspension stated is transferred in evaporating dish, is placed in 4h in 70~100 DEG C of baking oven, and rGO@MoS are made after evaporating solvent2/
PVDF composite materials.
The rGO@MoS2In/PVDF composite materials, rGO@MoS2The mass fraction of particle is 2.5~30wt%.
Embodiment 1：
The first step prepares rGO@MoS2Particle.
By graphene oxide GO and molybdenum disulfide with mass ratio for 2:1, gross mass is that 60mg is dissolved in 60mL water, ultrasonic 1h
So that the two is uniformly mixed, forms the first mixed liquor.First mixed liquor is placed in 90 DEG C of oil baths, after 10min, 32 μ L hydrations are added
Hydrazine reacts 2h.Last ultrasound 3h again.By the product centrifugation after ultrasound, washed successively with water and ethyl alcohol, it is dry, it is equal to obtain dispersion
Even rGO@MoS2Particle.Its pattern is as shown in Figure 1, molybdenum disulphide particles are uniformly dispersed in rGO and soilless sticking phenomenon.
Second step, the rGO@MoS of 5wt%2The preparation of/PVDF.
By the rGO@MoS that the first step is made2Particle is with PVDF with mass ratio for 1：19, gross mass weighs for 0.2g.
PVDF is dissolved in 30mL n,N-Dimethylformamide, ultrasound is until obtain transparent mixed liquor.It will be load weighted
rGO@MoS2Particle is dissolved in above-mentioned transparent mixed liquor, and mechanical agitation obtains black suspension.The black suspension is turned
Enter in evaporating dish, rGO@MoS are made after 4h evaporation solvents are placed in 70 DEG C of baking oven2/ PVDF composite materials.
Using pressure sintering to the 5wt%rGO@MoS2/ PVDF composite materials carry out tabletting, and coaxial method is used in combination to be inhaled
Wave is tested.Test results are shown in figure 2, passes through theoretical calculation, it has been found that when thickness changes in 1~5mm, reflection loss is minimum
For -43.1dB, corresponding sheeting thickness is 2mm, and frequency 14.48GHz shows optimal absorbing property.Wherein reflection loss
Frequency range less than -10dB is 3.6~18GHz, shows wideband absorption.
Embodiment 2：
The rGO@MoS of 25wt%2The preparation of/PVDF composite materials.
The first step prepares rGO@MoS2Particle.
By graphene oxide GO and molybdenum disulfide with mass ratio for 1:1, gross mass is that 60mg is dissolved in 60mL water, ultrasonic 1h
So that the two is uniformly mixed, forms the first mixed liquor.First mixed liquor is placed in 90 DEG C of oil baths, after 10min, 32 μ L hydrations are added
Hydrazine reacts 2h.Last ultrasound 3h again.By the product centrifugation after ultrasound, washed successively with water and ethyl alcohol, it is dry, it is equal to obtain dispersion
Even rGO@MoS2Particle.Its pattern is as shown in Figure 1, molybdenum disulphide particles are uniformly dispersed in rGO and soilless sticking phenomenon.
Second step, by rGO@MoS made from the first step2Particle is 0.2g, mass ratio 1 with gross mass with PVDF：3 carry out
It weighs.
PVDF is dissolved in 30mL n,N-Dimethylformamide, ultrasound is until obtain transparent mixed liquor.It will be load weighted
rGO@MoS2Material is dissolved in above-mentioned transparent mixed liquor, and mechanical agitation obtains black suspension.The black suspension of preparation is turned
Enter in evaporating dish, the rGO@MoS made after 4h evaporation solvents are placed in 70 DEG C of baking oven2/ PVDF composite materials.
Using pressure sintering to prepared 25wt%rGO@MoS2/ PVDF composite materials carry out tabletting, and coaxial method is used in combination to protect
S parameter is deposited to calculate shielding properties.Its shielding properties is as shown in Figure 3.From Fig. 3 A~3C it is found that working as rGO@MoS2/ PVDF contents
For the shielding properties for showing optimal when 25wt%, total shield effectiveness value maximum can reach 27.9dB.It is analyzed by calculating
It is to be reflected to go out most of electromagnetic wave to be absorbed without.
Using process conditions and technological parameter same as Example 1, rGO@MoS are prepared respectively2Content be
The rGO@MoS of 2.5wt%, 5.0wt%, 10wt%, 20wt%, 25wt%, 30wt%2/ PVDF composite materials carry out reality to it
It applies shielding properties shown in example 2 to test, as a result show as shown in fig.3 a 3 c.The shielding properties SE of the composite materialTotal
Increase with the increase of frequency, with rGO@MoS2The increase of content is substantially in rising trend, as rGO@MoS2Content be
When 25wt%, SETotalValue maximum up to 27.9dB.Electro-magnetic wave absorption efficiency SE has been calculated in weAAnd reflection performance
SER.It was found that SEAWith the variation relation and SE of frequency, contentTotalIt is identical.rGO@MoS2Content be 25wt% when, show most
Excellent absorbent properties, wherein SEAValue maximum up to 24.3dB.And reflection performance SERDo not become significantly with the content
Law.It is to be reflected that value by analyzing three, which can show that most of electromagnetic wave is absorbed without,.
Claims (5)
1. with the composite material for inhaling wave or capability of electromagnetic shielding, it is characterised in that：The composite material includes rGO@MoS2Grain
Son and PVDF, the rGO@MoS2The mass fraction of particle in the composite is 2.5~30wt%；By adjusting described
Mass fraction can adjust the suction wave or capability of electromagnetic shielding of the composite material；The rGO@MoS2Particle be by with
Lower step is prepared：
The first step, by graphene oxide GO and MoS2With mass ratio for 1:1~4:1, it is dissolved in deionized water, 1~2h of ultrasound makes two
Person is mixed into the first mixed liquor；
First mixed liquor is placed in 85~95 DEG C of oil baths by second step, and after 5~10min, hydrazine hydrate is added, reacts 2~3h；Most
2~4h of ultrasound again afterwards；
Third walks, and the product after ultrasound is centrifuged, is washed successively with water and ethyl alcohol, dry, obtains finely dispersed rGO@MoS2Grain
Son.
2. according to claim 1 have the composite material for inhaling wave or capability of electromagnetic shielding, it is characterised in that：When described
When mass fraction is 5wt%, the composite material has absorbing property；It is described when the mass fraction is 25wt%
Composite material have shielding properties.
3. according to claim 1 have the composite material for inhaling wave or capability of electromagnetic shielding, it is characterised in that：The GO with
MoS2Mass ratio be 2:1.
4. the preparation method with the composite material for inhaling wave or capability of electromagnetic shielding, it is characterised in that：
The first step, by graphene oxide GO and MoS2With mass ratio for 1:1~4:1, it is dissolved in deionized water, 1~2h of ultrasound makes two
Person is mixed into the first mixed liquor；
First mixed liquor is placed in 85~95 DEG C of oil baths by second step, and after 5~10min, hydrazine hydrate is added, reacts 2~3h；Most
2~4h of ultrasound again afterwards；
Third walks, and the product after ultrasound is centrifuged, is washed successively with water and ethyl alcohol, dry, obtains finely dispersed rGO@MoS2Grain
Son；
PVDF is dissolved in 30mL n,N-Dimethylformamide by the 4th step, and ultrasound is until obtain the second transparent mixed liquor；
5th step, by rGO@MoS2Particle is dissolved in above-mentioned second mixed liquor, and mechanical agitation obtains black suspension；It will be described
Black suspension is transferred in evaporating dish, is placed in 4h in 70~100 DEG C of baking oven, and rGO@MoS are made after evaporating solvent2/ PVDF is multiple
Condensation material, rGO@MoS2The mass fraction of particle is 2.5~30wt%.
5. the preparation method with the composite material for inhaling wave or capability of electromagnetic shielding according to claim 4, feature exist
In：The amount that hydrazine hydrate is added is the 0.05% of deionized water volume.
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| CN107812529B (en) * | 2017-10-30 | 2019-12-31 | 江苏大学 | Composite material photocatalyst and preparation method and application thereof |
| CN108360251A (en) * | 2018-01-30 | 2018-08-03 | 东莞市联洲知识产权运营管理有限公司 | A kind of surface is carbonization policrystalline silicon shell core suction wave particle of graphene and preparation method thereof and the application in textile finishing |
| CN108559249A (en) * | 2018-04-27 | 2018-09-21 | 南京恒新新材料有限公司 | A kind of graphene modified molybdenum disulfide wave absorbing agent and preparation method thereof |
| CN109082264B (en) * | 2018-07-04 | 2021-05-04 | 南京理工大学 | MoS2Application of/RGO composite material |
| CN108986961A (en) * | 2018-07-11 | 2018-12-11 | 常州凌天达传输科技有限公司 | A kind of polyvinylidene fluoride diene insulation electromagnetism filtered electrical cable and processing method |
| CN109943285B (en) * | 2019-04-16 | 2021-09-17 | 贵州大学 | High-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-composite and synthesis method thereof |
| CN110255536A (en) * | 2019-06-24 | 2019-09-20 | 王坤 | Composite material and preparation method with absorbing property and electromagnetic shielding performance |
| CN112063365B (en) * | 2020-09-04 | 2021-06-01 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
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| CN102604275B (en) * | 2012-03-07 | 2014-06-11 | 浙江工业大学 | Polyvinylidene fluoride/graphene composite and preparation method thereof |
| CN103951916B (en) * | 2014-04-29 | 2016-03-02 | 南昌航空大学 | Polyvinylidene difluoride (PVDF) composite wave-suction material that a kind of RGO/ ferric oxide is filled and preparation method thereof |
| CN105062417B (en) * | 2015-07-15 | 2017-07-21 | 北京新怡源环保科技有限公司 | A kind of organo-mineral complexing nanometer microwave absorbing material and preparation method thereof |
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