CN106398056A - Composite material with excellent wave absorption and electromagnetic shielding performances and preparation method thereof - Google Patents
Composite material with excellent wave absorption and electromagnetic shielding performances and preparation method thereof Download PDFInfo
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- CN106398056A CN106398056A CN201610803874.XA CN201610803874A CN106398056A CN 106398056 A CN106398056 A CN 106398056A CN 201610803874 A CN201610803874 A CN 201610803874A CN 106398056 A CN106398056 A CN 106398056A
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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 composite material with excellent wave absorption and electromagnetic shielding performances and a preparation method thereof, and belongs to the technical field of nano composite materials and preparation thereof. The composite material comprises rGO@MoS2 particles and PVDF, and the mass fraction of the rGO@MoS2 particles in the composite material is 2.5wt% to 30wt%. When the mass fraction is 5wt%, the composite material has wave absorption performance; and when the mass fraction is 25%, the composite material has shielding performance. The composite material provided by the invention is simple in preparation technology, molybdenum disulfide nanoparticles are stable, and the success rate of being compounded with oxidized graphene is extremely high, and the composite material is expected to be produced in a large scale; and the composite material provided by the invention has excellent wave absorption and electromagnetic shielding performances at the same time.
Description
Technical field
The invention belongs to nano composite material and its preparing technical field are and in particular to a kind of have excellent suction and involve electricity
Composite of magnetic shield performance and preparation method thereof.
Background technology
In the last few years, with the fast development of electronic equipment, electromagnetic wave as Information Communication carrier in military, boat
Empty space flight, the field such as civilian are extensively applied.However, electromagnetic wave but brings problems, such as electromagnetic interference, electromagnetic radiation etc.,
These all bring huge challenge to the healthy of people.
Interface impedance and energy loss by radiation are two key factors determining absorbing material.The performance of absorbing material is situated between
Electric value ε, magnetic permeability value μ and conductivity value δ impact, these parameters are the structure of wave absorbing agent and the reflection directly perceived of performance.Scientific research work
Authors pass through to adjust electrical conductivity, dielectric constant and the magnetic permeability value of material in the hope of low interface impedance and high lossy microwave.At present,
The absorbing property of the materials such as metal dust, pottery, ferrite has been studied, but most is due to density
Greatly, unstable etc. and be unable to practical application.
Electromagnetic shielding is suppression interference, realizes one of effective means of electromagnetic protection.When electromagnetic radiation is by air directive screen
When covering material, reflection, refraction effect can be produced on the surface of material, in material internal, multiple reflections phenomenon can occur.Electromagnetic screen
Cover and exactly using material, the reflection of electromagnetic radiation and refraction effect are realized suppressing the purpose of radiation.Shield effectiveness SE is to weigh
The factor of material capability of electromagnetic shielding, it includes absorption efficiency SE of shielding materialA, the reflection performance SE on shield surfaceRAnd screen
Cover multiple reflections efficiency SE in internal portionM.Reflection is relevant with the impedance matching of air and material, absorbs and may be considered electromagnetic wave
Energy attenuation in the material, multiple reflections represent the scattering effect that material internal inhomogeneities are led to, and it mainly occurs
Internally in the material at large area interface, such as porous material, mesh material etc..
Compared based on the electromagnetic shielding material of metal with traditional, graphene conductive macromolecular material is due to light weight, anti-corruption
Erosion, people are enjoyed the advantages of processing technique is simple, surface area is big, dielectric radio is high to pay close attention to.However, the electric conductivity of pure Graphene and electricity
Magnetic property can not meet impedance matching due to Tai Gao, and it is combined with other materials and is studied by therefore people.Molybdenum bisuphide
It is a kind of semi-conducting material, there is high electron mobility, in electro-catalysis, photocatalysis, battery, biology, sensing and electronic equipment
It is widely used in field.
Content of the invention
It is an object of the invention to overcome current material only to have single absorbing property, or capability of electromagnetic shielding is not
Foot, there is provided a kind of can have the composite that excellent suction involves capability of electromagnetic shielding simultaneously, and that is, described composite has
It is improved and inhale ripple amount or the purposes of widening frequency absorption section it is also possible to so that major part electromagnetic wave is absorbed without is to be reflected.
What the present invention provided has the composite that excellent suction involves capability of electromagnetic shielding, and described composite includes
rGO@MoS2Particle and PVDF, described rGO@MoS2Particle mass fraction in the composite is 2.5～30wt%.Work as institute
When the mass fraction stated is 5wt%, described composite has absorbing property；When described mass fraction is 25wt%,
Described composite has shielding propertiess.
Described has the preparation method that excellent suction involves the composite of capability of electromagnetic shielding, comprises 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, ultrasonic 1～
2h makes the two be mixed into the first mixed liquor.
Preferably, GO and MoS2Mass ratio be 2:1.
Second step, the first mixed liquor is placed in 85～95 DEG C of oil baths, after 5～10min, add hydrazine hydrate, reaction 2～
3h.Last ultrasonic again 2～4h.
3rd step, will be ultrasonic after product centrifugation, successively use water and washing with alcohol, be dried, obtain finely dispersed rGO@
MoS2Particle.
4th step, PVDF (Kynoar) is dissolved in 30mL DMF, ultrasonic transparent up to obtaining
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 proceeds in evaporating dish, is placed in 4h in 70～100 DEG C of baking oven, and rGO@MoS is obtained after evaporation solvent2/
PVDF composite.
Described rGO@MoS2In/PVDF composite, rGO@MoS2The mass fraction of particle is 2.5～30wt%.Work as institute
When the mass fraction stated is 5wt%, described composite has absorbing property；When described mass fraction is 25wt%,
Described composite has shielding propertiess.
Compared with existing absorbing material, the composite of the present invention has some advantage following：
(1) composite material preparation process that the present invention provides is simple, and molybdenum bisuphide only just can equably be divided by ultrasonic
It is dispersed in rGO and need not carry out other process.
(2) required molybdenum disulfide nano ball in the composite that the present invention provides is stable, and is combined with graphene oxide
Success rate very high, be expected to produce in a large number.
(3), after the absorbing material of present invention preparation is mixed with PVDF, not only drastically increase the suction ripple amount of material, and
Broaden frequency absorption section, therefore improve the absorbing property of material.
(4) composite that the present invention provides has excellent suction simultaneously and involves capability of electromagnetic shielding.
(5) preparation process of the composite that the present invention provides is most is physical method, easy and simple to handle, takes few, power consumption
Few, and without using other chemical reagent thus accomplishing environmental protection.
Brief description
Fig. 1 is the rGO@MoS of preparation in the embodiment of the present invention 12Scanning electron microscope (SEM) picture of particle；
The 5.0wt%rGO@MoS that Fig. 2 is prepared for the present invention2Reflection loss curve chart under/PVDF 1～5mm thickness；
Fig. 3 A～3C is respectively the 25.0wt%rGO@MoS of present invention preparation2The SE of/PVDF compositeTotal、SEAWith
SERValue is with frequency variation relation curve.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and examples.
The present invention provide a kind of there is excellent suction involve composite of capability of electromagnetic shielding and preparation method thereof, described
Composite include rGO@MoS2Particle and PVDF, described rGO@MoS2Particle mass fraction in the composite is 2.5
～30wt%.When described mass fraction is 5wt%, described composite has absorbing property；When described quality is divided
When number is for 25wt%, described composite has shielding propertiess.
Above-mentioned have the rGO@MoS that excellent suction involves capability of electromagnetic shielding2The preparation method of/PVDF composite, bag
Include following steps：
The first step, by GO and MoS2With mass ratio for 1:1～4:1, it is dissolved in deionized water, ultrasonic 1～2h makes the two mix
Close and uniformly become the first mixed liquor.
Second step, the first mixed liquor is placed in 85～95 DEG C of oil baths, after 5～10min, add hydrazine hydrate, reaction 2～
3h.Last ultrasonic again 2～4h.The amount wherein adding hydrazine hydrate is the 0.05% of deionized water volume.
3rd step, will be ultrasonic after product centrifugation, successively use water and washing with alcohol, be dried, obtain finely dispersed rGO@
MoS2Particle.
4th step, PVDF is dissolved in 30mLN, in dinethylformamide, ultrasonic 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 proceeds in evaporating dish, is placed in 4h in 70～100 DEG C of baking oven, and rGO@MoS is obtained after evaporation solvent2/
PVDF composite.
Described rGO@MoS2In/PVDF composite, rGO@MoS2The mass fraction of particle is 2.5～30wt%.
Embodiment 1：
The first step, prepares rGO@MoS2Particle.
By graphene oxide GO with molybdenum bisuphide with mass ratio for 2:1, gross mass is dissolved in 60mL water for 60mg, ultrasonic 1h
Make the two mix homogeneously, form the first mixed liquor.First mixed liquor is placed in 90 DEG C of oil baths, after 10min, adds 32 μ L hydrations
Hydrazine, reacts 2h.Last ultrasonic again 3h.Product centrifugation after will be ultrasonic, uses water and washing with alcohol successively, is dried, and obtains dispersion all
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 rGO@MoS made for the first step2Particle and PVDF are with mass ratio for 1：19, gross mass weighs for 0.2g.
PVDF is dissolved in 30mL DMF, ultrasonic until obtain transparent mixed liquor.Will be load weighted
rGO@MoS2Particle is dissolved in above-mentioned transparent mixed liquor, and mechanical agitation obtains black suspension.Described black suspension is turned
Enter in evaporating dish, after placing 4h evaporation solvent in 70 DEG C of the baking oven, rGO@MoS is obtained2/ PVDF composite.
Using pressure sintering to described 5wt%rGO@MoS2/ PVDF composite carries out tabletting, and is inhaled with coaxial method
Ripple is tested.Test result is as shown in Fig. 2 changed in 1～5mm it has been found that working as thickness by Theoretical Calculation, reflection loss is minimum
For -43.1dB, corresponding sheeting thickness is 2mm, and frequency is 14.48GHz, shows the absorbing property of optimum.Wherein reflection loss
Frequency range less than -10dB is 3.6～18GHz, shows wideband and absorbs.
Embodiment 2：
The rGO@MoS of 25wt%2The preparation of/PVDF composite.
The first step, prepares rGO@MoS2Particle.
By graphene oxide GO with molybdenum bisuphide with mass ratio for 1:1, gross mass is dissolved in 60mL water for 60mg, ultrasonic 1h
Make the two mix homogeneously, form the first mixed liquor.First mixed liquor is placed in 90 DEG C of oil baths, after 10min, adds 32 μ L hydrations
Hydrazine, reacts 2h.Last ultrasonic again 3h.Product centrifugation after will be ultrasonic, uses water and washing with alcohol successively, is dried, and obtains dispersion all
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 that the first step is obtained2, with gross mass as 0.2g, mass ratio is 1 for particle and PVDF：3 are carried out
Weigh.
PVDF is dissolved in 30mL DMF, ultrasonic until obtain transparent mixed liquor.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, place the rGO@MoS of system after 4h evaporation solvent in 70 DEG C of the baking oven2/ PVDF composite.
Using pressure sintering to prepared 25wt%rGO@MoS2/ PVDF composite carries out tabletting, and is protected with coaxial method
Deposit S parameter to calculate shielding propertiess.Its shielding properties is as shown in Figure 3.Knowable to Fig. 3 A～3C, as rGO@MoS2/ PVDF content
The shielding propertiess of optimum are shown, total shield effectiveness value maximum can reach 27.9dB during for 25wt%.Analyzed by calculating
Go out most of electromagnetic wave to be absorbed without is to be reflected.
Using process conditions same as Example 1 and technological parameter, prepare rGO@MoS respectively2Content be
The rGO@MoS of 2.5wt%, 5.0wt%, 10wt%, 20wt%, 25wt%, 30wt%2/ PVDF composite, carries out reality to it
Apply the shielding propertiess test shown in example 2, result shows as shown in fig.3 a 3 c.Shielding propertiess SE of described compositeTotal
Increase with the increase of frequency, with rGO@MoS2The increase of content is substantially in rising trend, as rGO@MoS2Content be
During 25wt%, SETotalValue maximum up to 27.9dB.We have calculated electro-magnetic wave absorption efficiency SEAAnd reflection performance
SER.Find SEAWith frequency, the variation relation of content and SETotalIdentical.rGO@MoS2Content be 25wt% when, show
Excellent absorbent properties, wherein SEAValue maximum up to 24.3dB.And reflection performance SERAnd significantly do not become with described content
Law.Can show that most of electromagnetic wave is absorbed without by the value analyzing three is to be reflected.
Claims (6)
1. have inhale involve capability of electromagnetic shielding composite it is characterised in that：Described composite includes rGO@MoS2Grain
Son and PVDF, described rGO@MoS2Particle mass fraction in the composite is 2.5～30wt%；Described by adjustment
Mass fraction, the suction that can adjust described composite involves capability of electromagnetic shielding.
2. according to claim 1 have inhale involve capability of electromagnetic shielding composite it is characterised in that：When described
When mass fraction is 5wt%, described composite has absorbing property；When described mass fraction is 25wt%, described
Composite there are shielding propertiess.
3. according to claim 1 have inhale involve capability of electromagnetic shielding composite it is characterised in that：Described
rGO@MoS2Particle is through the following steps that prepare：
The first step, by graphene oxide GO and MoS2With mass ratio for 1:1～4:1, it is dissolved in deionized water, ultrasonic 1～2h makes two
Person is mixed into the first mixed liquor；
Second step, the first mixed liquor is placed in 85～95 DEG C of oil baths, after 5～10min, adds hydrazine hydrate, reacts 2～3h；?
Ultrasonic 2～4h more afterwards；
3rd step, will be ultrasonic after product centrifugation, successively use water and washing with alcohol, be dried, obtain finely dispersed rGO@MoS2Grain
Son.
4. according to claim 1 have inhale involve capability of electromagnetic shielding composite it is characterised in that：Described GO with
MoS2Mass ratio be 2:1.
5. have inhale involve capability of electromagnetic shielding composite preparation method 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, ultrasonic 1～2h makes two
Person is mixed into the first mixed liquor；
Second step, the first mixed liquor is placed in 85～95 DEG C of oil baths, after 5～10min, adds hydrazine hydrate, reacts 2～3h；?
Ultrasonic 2～4h more afterwards；
3rd step, will be ultrasonic after product centrifugation, successively use water and washing with alcohol, be dried, obtain finely dispersed rGO@MoS2Grain
Son；
4th step, PVDF is dissolved in 30mL DMF, ultrasonic 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；Will be described
Black suspension proceeds in evaporating dish, is placed in 4h in 70～100 DEG C of baking oven, and rGO@MoS is obtained after evaporation solvent2/ PVDF is multiple
Condensation material, rGO@MoS2The mass fraction of particle is 2.5～30wt%.
6. according to claim 5 have the preparation method inhaling the composite involving capability of electromagnetic shielding, and its feature exists
In：The amount adding hydrazine hydrate is the 0.05% of deionized water volume.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107812529A (en) * | 2017-10-30 | 2018-03-20 | 江苏大学 | A kind of composite material photocatalyst and preparation method and application |
| 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 |
| 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 |
| CN109082264A (en) * | 2018-07-04 | 2018-12-25 | 南京理工大学 | MoS2The application of/RGO composite material |
| CN109943285A (en) * | 2019-04-16 | 2019-06-28 | 贵州大学 | A kind of high-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-complex and its synthetic method |
| CN110255536A (en) * | 2019-06-24 | 2019-09-20 | 王坤 | Composite material and preparation method with absorbing property and electromagnetic shielding performance |
| CN112063365A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107812529A (en) * | 2017-10-30 | 2018-03-20 | 江苏大学 | A kind of composite material photocatalyst and preparation method and application |
| 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 |
| CN109082264A (en) * | 2018-07-04 | 2018-12-25 | 南京理工大学 | MoS2The application of/RGO composite material |
| 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 |
| CN109943285A (en) * | 2019-04-16 | 2019-06-28 | 贵州大学 | A kind of high-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-complex and its synthetic 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 |
| CN112063365A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| 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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