CN106659105A - Wave-absorbing thin film and preparation method thereof - Google Patents

Wave-absorbing thin film and preparation method thereof Download PDF

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Publication number
CN106659105A
CN106659105A CN201710006188.4A CN201710006188A CN106659105A CN 106659105 A CN106659105 A CN 106659105A CN 201710006188 A CN201710006188 A CN 201710006188A CN 106659105 A CN106659105 A CN 106659105A
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China
Prior art keywords
thin film
wave absorbing
absorbing thin
preparation
hydrophilic
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CN201710006188.4A
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CN106659105B (en
Inventor
李永峰
巫家业
段永丽
傅婧怡
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01QANTENNAS, i.e. RADIO AERIALS
    • H01Q17/00Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems

Abstract

The invention provides a wave-absorbing thin film and a preparation method thereof. The preparation method includes: dissolving hydrophilic graphene and hydrophilic carbon nanotubes into water according to the mass ratio of 2:1, and performing ultrasonic treatment for 1-2 hours to obtain mixed liquid, wherein the mass sum of the hydrophilic graphene and the hydrophilic carbon nanotubes is 0.1-1wt% of the mass of the water; adding the mixed liquid into a polyethylene solution with the mass concentration being 1-12%, stirring for 0.5-2 hours, and drying under 40-80 DEG C and -0.01-0.01MPa for 24-48 hours to obtain the wave-absorbing thin film. The wave-absorbing thin film prepared by the method has wave-absorbing performance and certain toughness.

Description

A kind of wave absorbing thin film and preparation method thereof
Technical field
The present invention relates to a kind of wave absorbing thin film, more particularly to one kind is prepared by Graphene, CNT, polyvinyl alcohol Wave absorbing thin film, belong to technical field of material.
Background technology
Absorbing material is divided into powder body material and macromolecular material by material shape.Wherein, powder body material be prepare it is various micro- The material of form is seen, absorbing property is good, but material is difficult to apply.Macromolecular material be using different process by different macromolecules and Filler mixes, and is easy to application, but complex forming technology.
The magnetic conductivity and electrical conductivity of PVA is all very low, with very weak absorbing property, with stronger wave transparent performance, and can be with As absorbing material matrix.
Absorbing material based on PVAC polyvinylalcohol prepared by conventional method is mostly with redox graphene rGO as base Matter is added in PVA, shortcoming be prepare rGO method it is loaded down with trivial details and the cycle is long, the disposable amount for preparing is also few.
The content of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to provide it is a kind of have hydrophily, certain toughness and The simple extinction film of preparation method.
In order to realize above-mentioned technical purpose, the invention provides a kind of preparation method of wave absorbing thin film, the wave absorbing thin film Preparation method is comprised the following steps:
By hydrophilic Graphene and hydrophilic CNT with 2:1 mass ratio is soluble in water, ultrasonic 1h-12h, is mixed Close liquid, wherein, hydrophilic Graphene and the quality sum of hydrophilic CNT for the quality of water 0.1wt%-1wt%;
To mass concentration to add the mixed liquor in the polyethylene solution of 1%-12%, 0.5h-2h, 40 DEG C of -9- are stirred 80 DEG C, be dried 24h-48h under -0.01MPa to 0.01MPa, obtain wave absorbing thin film.
In the preparation method of the wave absorbing thin film of the present invention, it is preferable that the hydrophilic Graphene of employing is that Graphene exists Ball milling 4h-48h is obtained under the rotating speed of 400rpm-2000rpm.
It is highly preferred that using hydrophilic Graphene be by Graphene under the rotating speed of 500rpm ball milling 12h obtain.
In the preparation method of the wave absorbing thin film of the present invention, it is preferable that the hydrophilic CNT of employing is by carbon nanometer Pipe ball milling 4h-48h under the rotating speed of 400rpm-2000rpm is obtained.
It is highly preferred that using hydrophilic CNT be by CNT under the rotating speed of 500rpm ball milling 12h obtain 's.
In the preparation method of the wave absorbing thin film of the present invention, it is preferable that by hydrophilic Graphene and hydrophilic CNT After soluble in water, the time of ultrasound is 2h.
In the preparation method of the wave absorbing thin film of the present invention, it is preferable that the mass concentration of polyethylene solution is 10%.
In the preparation method of the wave absorbing thin film of the present invention, it is preferable that add in polyethylene solution after mixed liquor, stirring 30min。
The present invention wave absorbing thin film preparation method in, it is preferable that baking temperature be 60 DEG C, drying pressure for- 0.05MPa。
In the preparation method of the wave absorbing thin film of the present invention, it is preferable that drying time is 24h.
Present invention also offers a kind of wave absorbing thin film, the wave absorbing thin film is the preparation method system by above-mentioned wave absorbing thin film For what is obtained.
In the wave absorbing thin film of the present invention, it is preferable that the wall thickness of the wave absorbing thin film is 0.1mm-2mm.
The wave absorbing thin film of the present invention can be used in electromagnetic shielding and electromagnetic absorption, with good absorbing property and machine Tool performance (toughness).
The preparation method of the wave absorbing thin film of the present invention overcomes the scattering problem of Graphene and CNT, to Graphene and CNT is pre-processed, and obtains hydrophilic Graphene and CNT, makes hydrophilic Graphene and CNT uniform In being distributed to polyvinyl alcohol (PVA) aqueous solution.
The preparation method of the wave absorbing thin film of the present invention prepares hydrophilic graphene and CNT by ball-milling method, prepares week Phase is short, and the disposable yield for preparing is big.
Wave absorbing thin film prepared by the preparation method of the wave absorbing thin film of the present invention is also equipped with except possessing certain absorbing property Certain toughness, can be cut into any shape.
Polyvinyl alcohol (PVA) is a kind of hydrophilic macromolecule, and polyvinyl alcohol water solution can be obtained by vacuum drying Polyvinyl alcohol film.Graphene and CNT itself do not possess hydrophily, it is impossible to polyvinyl alcohol.The suction ripple of the present invention The preparation method of film prepares hydrophilic Graphene and CNT by ball milling, by hydrophilic Graphene and CNT according to Certain proportion is added in polyvinyl alcohol water solution, and vacuum drying obtains graphene/carbon nano-tube/polyvinyl alcohol film, obtains Film possess certain absorbing property, and possess certain toughness, be easy to practical application.
In addition, what the preparation method of the present invention adopted is nontoxic reagent, safe preparation process, environmental protection.
Description of the drawings
Fig. 1 is the absorbing property curve of the wave absorbing thin film in embodiment 1.
Fig. 2 is the tensile property curve of the wave absorbing thin film in embodiment 1.
Specific embodiment
In order to be more clearly understood to the technical characteristic of the present invention, purpose and beneficial effect, now to the skill of the present invention Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of wave absorbing thin film is present embodiments provided, it is prepared in accordance with the following steps:
Graphene 10g is weighed, is put in ball grinder, regulation rotational speed of ball-mill is 500rpm, sample 1 is taken out after 12 hours;
CNT 10g is weighed, is put in ball grinder, regulation rotational speed of ball-mill is 500rpm, sample 2 is taken out after 12 hours;
Mass 60mg of sample 1 is weighed, mass 30mg of sample 2 adds 100mL deionized waters, ultrasonic 2h;
Solution after above-mentioned ultrasound is added in the poly-vinyl alcohol solution that 100mL mass concentrations are 10%, magnetic agitation 30min
The solution that step 4 is obtained is poured in culture dish, is put into vacuum drying chamber, and it is 60 DEG C to adjust baking temperature, vacuum For -0.05MPa.
Culture dish is taken out after 24 hours, wave absorbing thin film is obtained.
The present embodiment has carried out absorbing property test to above-mentioned wave absorbing thin film, as a result as shown in Figure 1.Absorbing property test tool Body is followed the steps below:
The above-mentioned wave absorbing thin film of the present embodiment is made into external diameter 7mm, internal diameter 3.04mm, thickness 0.1- using punch device The donut of 2mm, using vector network analyzer its magnetic conductivity and electrical conductivity are measured, and are calculated further according to magnetic conductivity and electrical conductivity Its absorbing property.
The evaluation index of absorbing property is that the numerical value and absorption peak strength of the maximum absorption band (ordinate) that can be reached are little In frequency band (abscissa) width of -10dB.From figure 1 it appears that when thickness is 5mm, the suction ripple of the present embodiment is thin The absorption maximum peak intensity of film has reached -37dB, and the frequency bandwidth less than -10dB is 2GHz, little when thickness is 2mm It is 7.7GHz in the frequency bandwidth of -10dB, the wave absorbing thin film for illustrating the present embodiment has stronger wave-absorbing effect.
Also tensile property test is carried out to the wave absorbing thin film of the present embodiment, as a result as shown in Figure 2.Ordinate table in Fig. 2 Show the pulling force that the wave absorbing thin film of the present embodiment is subject in drawing process, abscissa represents its elongation.Can see, it is stretched The maximum pull being subject in journey is 39MPa, and elongation when sample ruptures has reached 106% or so, the bigger table of elongation at break Show that its toughness is better.
Above example illustrates, the film that obtains of preparation method of the wave absorbing thin film of the present invention possess certain wave absorbtion and Toughness, is easy to practical application.

Claims (10)

1. a kind of preparation method of wave absorbing thin film, it is characterised in that the preparation method of the wave absorbing thin film is comprised the following steps:
By hydrophilic Graphene and hydrophilic CNT with 2:1 mass ratio is soluble in water, ultrasonic 1h-12h, is mixed Liquid;Wherein, the quality sum of the hydrophilic Graphene and hydrophilic CNT is the 0.1wt%-1wt% of the quality of water;
To mass concentration to add the mixed liquor in the polyethylene solution of 1%-12%, 0.5h-2h is stirred, 40 DEG C -80 DEG C, - 24h-48h is dried under 0.01MPa to 0.01MPa, the wave absorbing thin film is obtained.
2. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that the hydrophilic Graphene is by stone Black alkene ball milling 4h-48h under the rotating speed of 400rpm-2000rpm is obtained.
3. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that the hydrophilic CNT be by CNT ball milling 4h-48h under the rotating speed of 400rpm-2000rpm is obtained.
4. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that by hydrophilic Graphene and hydrophilic After CNT is soluble in water, the time of ultrasound is 2h.
5. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that the quality of the polyethylene solution is dense Spend for 10%.
6. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that add in the polyethylene solution After mixed liquor, 30min is stirred.
7. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that baking temperature is 60 DEG C, is dried pressure Power is -0.05MPa.
8. the preparation method of wave absorbing thin film according to claim 1, it is characterised in that drying time is 24h.
9. a kind of wave absorbing thin film, it is characterised in that the wave absorbing thin film is by the wave absorbing thin film described in any one of claim 1-8 Preparation method prepare.
10. wave absorbing thin film according to claim 9, it is characterised in that the wall thickness of the wave absorbing thin film is 0.1mm-2mm.
CN201710006188.4A 2017-01-05 2017-01-05 A kind of wave absorbing thin film and preparation method thereof Active CN106659105B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325787A (en) * 2017-07-05 2017-11-07 中国石油天然气股份有限公司 A kind of hollow carbon nano-particle and the absorbing material prepared by it

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100330358A1 (en) * 2008-02-08 2010-12-30 Meijo Nano Carbon Co., Ltd. Carbon nanotube dispersion and utilization of same
CN103306132A (en) * 2012-03-15 2013-09-18 苏州捷迪纳米科技有限公司 Carbon nano tube fiber-graphene composite material and preparation method of the same
CN104495780A (en) * 2014-12-30 2015-04-08 浙江碳谷上希材料科技有限公司 Hydrophilic graphene-carbon nano-tube composite super-light elastic aerogel and preparation method thereof
CN105948029A (en) * 2016-05-09 2016-09-21 东华大学 Graphene roll/carbon nanotube composite aerogel material, preparation and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100330358A1 (en) * 2008-02-08 2010-12-30 Meijo Nano Carbon Co., Ltd. Carbon nanotube dispersion and utilization of same
CN103306132A (en) * 2012-03-15 2013-09-18 苏州捷迪纳米科技有限公司 Carbon nano tube fiber-graphene composite material and preparation method of the same
CN104495780A (en) * 2014-12-30 2015-04-08 浙江碳谷上希材料科技有限公司 Hydrophilic graphene-carbon nano-tube composite super-light elastic aerogel and preparation method thereof
CN105948029A (en) * 2016-05-09 2016-09-21 东华大学 Graphene roll/carbon nanotube composite aerogel material, preparation and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325787A (en) * 2017-07-05 2017-11-07 中国石油天然气股份有限公司 A kind of hollow carbon nano-particle and the absorbing material prepared by it
CN107325787B (en) * 2017-07-05 2021-01-29 中国石油天然气股份有限公司 Hollow carbon nano-particles and wave-absorbing material prepared from same

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