CN106659105B - A kind of wave absorbing thin film and preparation method thereof - Google Patents

A kind of wave absorbing thin film and preparation method thereof Download PDF

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Publication number
CN106659105B
CN106659105B CN201710006188.4A CN201710006188A CN106659105B CN 106659105 B CN106659105 B CN 106659105B CN 201710006188 A CN201710006188 A CN 201710006188A CN 106659105 B CN106659105 B CN 106659105B
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thin film
wave absorbing
absorbing thin
preparation
hydrophilic
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CN106659105A (en
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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 present invention provides a kind of wave absorbing thin films and preparation method thereof.For the preparation method of the wave absorbing thin film the following steps are included: hydrophilic graphene and hydrophilic carbon nanotube is soluble in water with the mass ratio of 2:1, ultrasonic 1h-12h obtains mixed liquor;The quality sum of hydrophilic graphene and hydrophilic carbon nanotube is the 0.1wt%-1wt% of the quality of water;The mixed liquor is added into the polyvinyl alcohol water solution that mass concentration is 1%-12%, stirs 0.5h-2h, and 40 DEG C -80 DEG C, dry -48h for 24 hours under -0.01MPa to 0.01MPa obtain wave absorbing thin film.The present invention also provides the wave absorbing thin films as made from above-mentioned preparation method.The wave absorbing thin film that preparation method through the invention is prepared has absorbing property 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 films, more particularly to one kind to be prepared by graphene, carbon nanotube, polyvinyl alcohol Wave absorbing thin film, belong to technical field of material.
Background technique
Absorbing material is divided into powder body material and high molecular 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.High molecular material be using different process by different macromolecules and Filler mixing, convenient for applying, but complex forming technology.
The magnetic conductivity and conductivity of PVA is all very low, has very weak absorbing property, has stronger wave transparent performance, can be with As absorbing material matrix.
The PVAC polyvinylalcohol of conventional method preparation is that the absorbing material of matrix is mostly using redox graphene rGO as base Matter is added in PVA, and disadvantage is that the method for preparing rGO is cumbersome and the period is long, and the amount disposably prepared is also few.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide one kind have hydrophily, certain toughness and The simple extinction film of preparation method.
In order to achieve the above technical purposes, the present invention provides a kind of preparation method of wave absorbing thin film, the wave absorbing thin film Preparation method the following steps are included:
Hydrophilic graphene and hydrophilic carbon nanotube is soluble in water with the mass ratio of 2:1, and ultrasonic 1h-12h is mixed Close liquid, wherein the quality sum of hydrophilic graphene and hydrophilic carbon nanotube is the 0.1wt%-1wt% of the quality of water;
The mixed liquor is added into the polyvinyl alcohol water solution that mass concentration is 1%-12%, stirs 0.5h-2h, 40 DEG C -9-80 DEG C, dry -48h for 24 hours under -0.01MPa to 0.01MPa, obtain wave absorbing thin film.
In the preparation method of wave absorbing thin film of the invention, it is preferable that the hydrophilic graphene of use is that graphene exists Ball milling 4h-48h is obtained under the revolving speed of 400rpm-2000rpm.
It is highly preferred that the hydrophilic graphene used is that ball milling 12h is obtained under the revolving speed of 500rpm by graphene.
In the preparation method of wave absorbing thin film of the invention, it is preferable that the hydrophilic carbon nanotube of use is by carbon nanometer Pipe ball milling 4h-48h under the revolving speed of 400rpm-2000rpm is obtained.
It is highly preferred that the hydrophilic carbon nanotube used is that ball milling 12h is obtained under the revolving speed of 500rpm by carbon nanotube 's.
In the preparation method of wave absorbing thin film of the invention, it is preferable that by hydrophilic graphene and hydrophilic carbon nanotube After soluble in water, the ultrasonic time is 2h.
In the preparation method of wave absorbing thin film of the invention, it is preferable that the mass concentration of polyvinyl alcohol water solution is 10%.
In the preparation method of wave absorbing thin film of the invention, it is preferable that after mixed liquor is added into polyvinyl alcohol water solution, Stir 30min.
In the preparation method of wave absorbing thin film of the invention, it is preferable that drying temperature be 60 DEG C, drying pressure be- 0.05MPa。
In the preparation method of wave absorbing thin film of the invention, it is preferable that drying time is for 24 hours.
The present invention also provides a kind of wave absorbing thin film, which is the preparation method system by above-mentioned wave absorbing thin film For what is obtained.
In wave absorbing thin film of the invention, it is preferable that the wall thickness of the wave absorbing thin film is 0.1mm-2mm.
Wave absorbing thin film of the invention can be used for being electromagnetically shielded in electromagnetic absorption, have good absorbing property and machine Tool performance (toughness).
The preparation method of wave absorbing thin film of the invention overcomes the dispersion of graphene and carbon nanotube, to graphene and Carbon nanotube is pre-processed, and hydrophilic graphene and carbon nanotube are obtained, and keeps hydrophilic graphene and carbon nanotube uniform It is distributed in polyvinyl alcohol (PVA) aqueous solution.
The preparation method of wave absorbing thin film of the invention prepares hydrophilic graphene and carbon nanotube, preparation week by ball-milling method Phase is short, and the yield disposably prepared is big.
The wave absorbing thin film of the preparation method preparation of wave absorbing thin film of the invention is also equipped in addition to having 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 is available by being dried in vacuo Polyvinyl alcohol film.Graphene and carbon nanotube itself do not have hydrophily, can not be with polyvinyl alcohol.Suction wave of the invention The preparation method of film prepares hydrophilic graphene and carbon nanotube by ball milling, by hydrophilic graphene and carbon nanotube according to Certain proportion is added in polyvinyl alcohol water solution, and vacuum drying obtains graphene/carbon nano-tube/polyvinyl alcohol film, obtains Film have certain absorbing property, and have certain toughness, be convenient for practical application.
In addition, what preparation method of the invention used is nontoxic reagent, safe preparation process, environmental protection.
Detailed description of the invention
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 which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
A kind of wave absorbing thin film is present embodiments provided, is prepared in accordance with the following steps:
Graphene 10g is weighed, is put into ball grinder, adjusting rotational speed of ball-mill is 500rpm, and sample 1 is taken out after 12 hours;
Carbon nanotube 10g is weighed, is put into ball grinder, adjusting rotational speed of ball-mill is 500rpm, and sample 2 is taken out after 12 hours;
1 mass 60mg of sample, 2 mass 30mg of sample are weighed, 100mL deionized water, ultrasonic 2h is added;
Solution after above-mentioned ultrasound is added in the polyvinyl alcohol water solution that 100mL mass concentration is 10%, magnetic force stirs Mix 30min
The solution that step 4 obtains pours into culture dish, is put into vacuum oven, and adjusting drying temperature is 60 DEG C, vacuum degree For -0.05MPa.
Culture dish is taken out after 24 hours, obtains wave absorbing thin film.
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 follows the steps below:
The above-mentioned wave absorbing thin film of the present embodiment is made into outer diameter 7mm, internal diameter 3.04mm, thickness 0.1- using punch device The concentric loop of 2mm measures its magnetic conductivity and conductivity using vector network analyzer, calculates further according to magnetic conductivity and conductivity Its absorbing property.
The evaluation index of absorbing property be attainable maximum absorption band (ordinate) numerical value and absorption peak strength it is small In frequency band (abscissa) width of -10dB.From figure 1 it appears that the suction wave of the present embodiment is thin when with a thickness of 5mm The absorption maximum peak intensity of film has reached -37dB, and the frequency bandwidth less than -10dB is 2GHz, small when with a thickness of 2mm It is 7.7GHz in the frequency bandwidth of -10dB, illustrates that the wave absorbing thin film of the present embodiment has stronger wave-absorbing effect.
Tensile property test also 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 that the pulling force that the wave absorbing thin film of the present embodiment is subject to during stretching, abscissa indicate its elongation.It can be seen that stretching The maximum pull being subject in journey is 39MPa, and elongation when sample is broken has reached 106% or so, the bigger table of elongation at break Show that its toughness is better.
Above embodiments explanation, the film that the preparation method of wave absorbing thin film of the invention obtains have certain wave absorbtion and Toughness is convenient for practical application.

Claims (8)

1. a kind of preparation method of wave absorbing thin film, which is characterized in that the preparation method of the wave absorbing thin film the following steps are included:
Hydrophilic graphene and hydrophilic carbon nanotube is soluble in water with the mass ratio of 2:1, and ultrasonic 1h-12h is mixed Liquid;Wherein, the quality sum of the hydrophilic graphene and hydrophilic carbon nanotube is the 0.1wt%-1wt% of the quality of water;
The mixed liquor is added into the polyvinyl alcohol water solution that mass concentration is 1%-12%, stirs 0.5h-2h, 40 DEG C -80 DEG C, dry -48h for 24 hours under -0.01MPa to 0.01MPa, obtain the wave absorbing thin film;
Wherein, the hydrophilic graphene is that ball milling 4h-48h is obtained under the revolving speed of 400rpm-2000rpm by graphene;
The hydrophilic carbon nanotube is that ball milling 4h-48h is obtained under the revolving speed of 400rpm-2000rpm by carbon nanotube.
2. the preparation method of wave absorbing thin film according to claim 1, which is characterized in that by hydrophilic graphene and hydrophilic After carbon nanotube is soluble in water, the ultrasonic time is 2h.
3. the preparation method of wave absorbing thin film according to claim 1, which is characterized in that the matter of the polyvinyl alcohol water solution Measuring concentration is 10%.
4. the preparation method of wave absorbing thin film according to claim 1, which is characterized in that in Xiang Suoshu polyvinyl alcohol water solution After mixed liquor is added, 30min is stirred.
5. the preparation method of wave absorbing thin film according to claim 1, which is characterized in that drying temperature is 60 DEG C, dry pressure Power is -0.05MPa.
6. the preparation method of wave absorbing thin film according to claim 1, which is characterized in that drying time is for 24 hours.
7. a kind of wave absorbing thin film, which is characterized in that the wave absorbing thin film is by wave absorbing thin film described in any one of claims 1-6 Preparation method be prepared.
8. wave absorbing thin film according to claim 7, which is characterized 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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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

Citations (3)

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Publication number Priority date Publication date Assignee Title
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

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US9181090B2 (en) * 2008-02-08 2015-11-10 Meijo Nano Carbon Co., Ltd. Carbon nanotube dispersion and utilization of same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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