CN106243379B - A kind of electromagnetic shielding foamed composite and preparation method based on graphene oxide and polymer - Google Patents
A kind of electromagnetic shielding foamed composite and preparation method based on graphene oxide and polymer Download PDFInfo
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- CN106243379B CN106243379B CN201610600217.5A CN201610600217A CN106243379B CN 106243379 B CN106243379 B CN 106243379B CN 201610600217 A CN201610600217 A CN 201610600217A CN 106243379 B CN106243379 B CN 106243379B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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Abstract
The present invention relates to a kind of electromagnetic shielding foamed composite and preparation method based on graphene oxide and polymer；Selecting has flexible foam of polymers, and after foam of polymers is impregnated in graphene oxide aqueous dispersions, dried, restoring, one layer of three-dimensional continuous graphite alkene membrane structure is formed between its foam framework and skeleton；Graphene film between skeleton is conducive to improve the reflecting surface of electromagnetic wave, is conducive to the absorption of electromagnetic wave；Pass through the compound and reduction of foam of polymers and graphene oxide, realize with flexible foam of polymers with high electromagnetic shielding performance graphene it is compound, the three-dimensional contiguous network structure of foam of polymers and graphene has ensured the maximization of mechanics and electromagnetic shielding performance, Repeated Compression 1000 times under 80% compression strain of obtained foamed composite, response rate is more than or equal to 95%, and electromagnet shield effect is more than or equal to 40dB.Combination process of the present invention is simple, can magnanimity production.
Description
Technical field
The present invention relates to a kind of preparation methods for having both high electromagnetic wave shielding and flexible foamed material, specifically
A kind of preparation method of graphene oxide and flexible polymer foamed composite.
Background technique
With the fast development of science and technology, mainframe computer, laptop and many other electronic devices are to people
The life of class brings great convenience, while also producing serious electromagnetic radiation, caused by electromagnetic pollution, electromagnetic interference give
High-precision electronic equipment and the physical and mental health of the mankind cause serious influence.In order to solve this problem, all kinds of high-performance gold
Belong to base electromagnetic screen material to be continuously developed.However, light and flexibility is also electromagnetism other than high electromagnetic shielding performance
Other two shielding important technical requirements, especially in aircraft, satellite, laptop, wearable electronic device etc.
Field.
In recent years using carbon fiber, carbon nanotube and graphene as the carbon material of representative, because having low-density, good conduction
Property and excellent mechanical property are widely used as the conductive additive of electromagnetic shielding composite material.However, in these composite materials
In, conductive additive is desultorily distributed in polymer matrix, and is separated by matrix, in order to obtain higher conductance ability
And electromagnetic shielding performance, it has to add a large amount of conductive additive in matrices of composite material to form good conductive mesh
Network, while this can also seriously affect the mechanical property of material.
Constructing three-dimensional continuous conduction network is a kind of important channel for reducing conductive additive.For this purpose, having three-dimensional continuous
The grapheme foam of structure is developed, and includes mainly two kinds of preparation methods, first is that the graphene based on metal foam template
Chemical vapor deposition, second is that the hydro-thermal self assembly based on graphene oxide.Chen etc. passes through chemical gaseous phase on nickel foam surface
Sedimentation prepares single-layer graphene, and nickel template is removed after cement-based powder material filling, and maximum electromagnet shield effect reaches 30dB
(Zongping Chen et al.Lightweight and flexible graphene foam composites for
high-performance electromagnetic interference shielding.Advanced Materials,
2013,25,1296-1300).However, such method it is high to equipment and technical requirements (accurately controlled under the conditions of 1000 DEG C carbon source and
Air-flow), it is difficult to realize inexpensive magnanimity preparation.Zhang etc. is prepared for graphene oxide foam by hydro-thermal self assembly, passes through tune
The chemical structure and pore structure of graphene surface are controlled, maximum electromagnet shield effect reaches 34dB (Yi Zhang et
al.Composition and structure control of ultralight graphene foam for high-
performance microwave absorption.Carbon,2016,105,438-447).Although having excellent electromagnetism
Shielding properties, the graphene oxide froth texture is fragile, cannot compress, limit its practical application.
In order to make foamed material have both flexibility and excellent electric conductivity, stone is loaded on the skeleton of open celled polymeric foam
The strategy of black alkene is developed, which has excellent conduction and flexible energy (Chao Wu et
al.Mechanically flexible and multifunctional polymer-based graphene foams for
elastic conductors and oil-water separators.Advanced Materials,2013,25,5658-
5662).However, graphene is only coated on the skeleton of foam of polymers, to incoming electromagnetic since the foam densities are low
The reflecting surface of wave is smaller, it is difficult to realize the effective reflection and absorption to incident electromagnetic wave, be unfavorable for the raising of electromagnetic shielding performance.
Therefore, the flexibility of polymer and the high-termal conductivity of graphene are made full use of, constructs special space structure, exploitation
One kind, which having both excellent electromagnetic shielding properties and flexible foamed composite, to be particularly important.
Summary of the invention
The present invention provides one for existing grapheme foam material flexibility deficiency and the lower defect of electromagnetic shielding performance
Kind has both the preparation method of excellent electromagnetic shielding properties and flexible foamed composite.
The invention adopts the following technical scheme:
One kind having both excellent electromagnetic shielding properties and flexible foamed composite (such as Fig. 1 (a))；It selects with flexible
The foam of polymers of property, after foam of polymers is impregnated in graphene oxide aqueous dispersions, dried, restoring, in its foam framework
And one layer of three-dimensional continuous graphite alkene membrane structure (such as Fig. 1 (b)) is formed between skeleton；Foam of polymers bone in the foamed composite
Frame has ensured the flexibility of composite material, and three-dimensional continuous graphene constructs three-dimensional conductive network (such as Fig. 1 (c)) on skeleton,
Graphene film between skeleton is conducive to improve the reflecting surface of electromagnetic wave, is conducive to the absorption (such as Fig. 1 (d)) of electromagnetic wave；It obtains
Foamed composite Repeated Compression 1000 times under 80% compression strain, response rate be more than or equal to 95%, electromagnetic shielding effect
40dB can be more than or equal to；
A kind of preparation method having both electromagnetic shielding performance and flexible foamed composite, steps are as follows:
1) preparation of graphene oxide aqueous dispersions: neutral graphene oxide aqueous dispersions are freeze-dried, are obtained
Graphene oxide powder is obtained, deionized water is added in graphene oxide powder, one is placed in cell disruptor in 20~200W function
3~20min is handled under rate, obtains the graphene oxide aqueous dispersions of mass fraction 0.05~3%；
2) foam of polymers is immersed in above-mentioned graphene oxide aqueous dispersions, repeatedly extruding foam of polymers makes to aoxidize
Graphene aqueous dispersions uniform adsorption is in the hole of foam of polymers, the quality of the foam of polymers and graphene oxide
Than being obtained after the above-mentioned foam of polymers for being adsorbed with graphene oxide aqueous dispersions is dried in vacuum drying oven for 9~99:1
Foamed composite based on graphene oxide；
3) the above-mentioned foamed composite based on graphene oxide is placed in the hydroiodic acid or matter of mass fraction 0.5~40%
Measure score 0.5~40% hydrazine hydrate solution in, at 60~120 DEG C flow back 0.5~3h, washed, dry after be based on
The foamed composite of redox graphene.
The foam of polymers is the open cell polymers such as polyurethane foam, polyimide foam or silicon rubber foam bubble
Foam.
The mass ratio of the foam of polymers and graphene oxide is 9~99:1.
It is described as follows:
(1) commercial product can be used in graphene oxide aqueous dispersions, can keep graphene oxide layer using freeze-drying
Dispersibility, can avoid the reunion of graphene oxide layer, help to obtain the graphene oxide aqueous dispersions of quantization, aoxidize stone
Black alkene in aqueous solution can be evenly dispersed because having the oxygen-containing groups such as great amount of hydroxy group, carboxyl；
(2) commercial product can be used in open celled polymeric foam, can be polyurethane, polyimides, silicon rubber etc.；
(3) after open celled polymeric foam oxide impregnation graphene aqueous dispersions, during drying, due to graphite oxide
There are Van der Waals force, graphene oxide is evenly coated on foam framework for alkene and foam of polymers skeleton, simultaneously because oxidation stone
There are huge interfacial tensions between black aqueous solution and skeleton, so that graphene oxide also forms film between foam framework
Structure, for graphene oxide after restoring and becoming graphene, graphene forms three-dimensional between the skeleton and skeleton of foam of polymers
Contiguous network structure, foam of polymers skeleton has ensured the flexibility of composite material in the foamed composite, three-dimensional on skeleton
Continuous graphene constructs three-dimensional conductive network, and the graphene film between skeleton is conducive to improve the reflecting surface of electromagnetic wave, has
Conducive to the absorption of electromagnetic wave.
By the compound and reduction of above step foam of polymers and graphene oxide, realize with flexible polymerization
Compound, the three-dimensional contiguous network structure of foam of polymers and graphene of object foam and the graphene with high electromagnetic shielding performance
The maximization for having ensured mechanics and electromagnetic shielding performance, obtained foamed composite Repeated Compression under 80% compression strain
1000 times, response rate is more than or equal to 95%, and electromagnet shield effect is more than or equal to 40dB.
Beneficial effects of the present invention: matrix material foam of polymers of the invention and graphene oxide are simple easy, and
Be commercially available, in the present invention combination process of foam of polymers and graphene it is simple, can magnanimity production, stone in foamed composite
The content demand of black alkene is low, and mechanics and electromagnetic shielding performance are better than other carbon foams.
Detailed description of the invention:
Fig. 1 is the macro-and micro-structure picture of foamed composite of the invention, and wherein Fig. 1 (a) is foam composite
Macroscopical picture of material, Fig. 1 (b) are the partial enlargement picture of foamed composite in Fig. 1 (a), and Fig. 1 (d) is the part of Fig. 1 (b)
Amplification picture shows that graphene forms membrane structure between foam framework, and Fig. 1 (c) is the partial enlargement picture of Fig. 1 (d), table
Bright graphene forms film on foam framework；
Fig. 2 is the electromagnetic shielding performance test result of foamed composite of the invention, and number 1 to 6 respectively corresponds implementation
The test result of example 1 to 6.
Specific embodiment
6 embodiments of the invention are given below, are that rather than model of the invention is limited to further explanation of the invention
It encloses.
Embodiment 1
Neutral graphene oxide aqueous dispersions are freeze-dried, graphene oxide powder are obtained, by the oxygen of 100mg
The deionized water of 20g is added in graphite alkene powder, and one is placed in cell disruptor handles 20min under 20W power, obtains quality
The graphene oxide aqueous dispersions of score 0.05%；Open-celled polyurethane foam is cut into the cubic block of 9.9g, is immersed in
In above-mentioned graphene oxide aqueous dispersions, repeatedly extruding polyurethane foam makes graphene oxide aqueous dispersions uniform adsorption in poly- ammonia
In the hole of ester foam, the mass ratio of the polyurethane foam and graphene oxide is 99:1, obtains base after vacuum dried
In the foamed composite of graphene oxide；The above-mentioned foamed composite based on graphene oxide is placed in mass fraction
In 0.5% hydrazine hydrate solution, flow back 3h at 60 DEG C, and the foam based on redox graphene is obtained after being washed, being dried
Composite material.Repeated Compression 1000 times under 80% compression strain of obtained foamed composite, response rate is more than or equal to
95%, its electromagnetic shielding performance is tested, as shown in Fig. 2, its electromagnet shield effect is more than or equal to 40dB.
Embodiment 2
Neutral graphene oxide aqueous dispersions are freeze-dried, graphene oxide powder are obtained, by the oxygen of 100mg
The deionized water of 20g is added in graphite alkene powder, and one is placed in cell disruptor handles 3min under 200W power, obtains quality
The graphene oxide aqueous dispersions of score 0.05%；Open-celled polyurethane foam is cut into the cubic block of 9.9g, is immersed in
In above-mentioned graphene oxide aqueous dispersions, repeatedly extruding polyurethane foam makes graphene oxide aqueous dispersions uniform adsorption in poly- ammonia
In the hole of ester foam, the mass ratio of the polyurethane foam and graphene oxide is 99:1, obtains base after vacuum dried
In the foamed composite of graphene oxide；The above-mentioned foamed composite based on graphene oxide is placed in mass fraction 1%
Hydrazine hydrate solution in, flow back 3h at 80 DEG C, after being washed, being dried obtain the foam composite based on redox graphene
Material.Repeated Compression 1000 times under 80% compression strain of obtained foamed composite, response rate are more than or equal to 96%, test
Its electromagnetic shielding performance, as shown in Fig. 2, its electromagnet shield effect is more than or equal to 42dB.
Embodiment 3
Neutral graphene oxide aqueous dispersions are freeze-dried, graphene oxide powder are obtained, by the oxygen of 100mg
The deionized water of 20g is added in graphite alkene powder, and one is placed in cell disruptor handles 10min under 100W power, obtains matter
Measure the graphene oxide aqueous dispersions of score 0.05%；Open-celled polyurethane foam is cut into the cubic block of 9.9g, is impregnated
In above-mentioned graphene oxide aqueous dispersions, repeatedly extruding polyurethane foam makes graphene oxide aqueous dispersions uniform adsorption poly-
In the hole of urethane foam, the mass ratio of the polyurethane foam and graphene oxide is 99:1, is obtained after vacuum dried
Foamed composite based on graphene oxide；The above-mentioned foamed composite based on graphene oxide is placed in mass fraction
In 40% hydrazine hydrate solution, flow back 0.5h at 120 DEG C, and the bubble based on redox graphene is obtained after being washed, being dried
Foam composite material.Repeated Compression 1000 times under 80% compression strain of obtained foamed composite, response rate is more than or equal to
95%, its electromagnetic shielding performance is tested, as shown in Fig. 2, its electromagnet shield effect is more than or equal to 42dB.
Embodiment 4
Neutral graphene oxide aqueous dispersions are freeze-dried, graphene oxide powder are obtained, by the oxygen of 100mg
The deionized water of 9.9g is added in graphite alkene powder, and one is placed in cell disruptor handles 20min under 80W power, obtains matter
Measure the graphene oxide aqueous dispersions of score 1%；Open-Cells Silicone Rubber Foam is cut into the cubic block of 5g, is immersed in above-mentioned
In graphene oxide aqueous dispersions, repeatedly extruding silicon rubber foam steeps graphene oxide aqueous dispersions uniform adsorption in silicon rubber
In the hole of foam, the mass ratio of the silicon rubber foam and graphene oxide is 50:1, obtains after vacuum dried and is based on oxygen
The foamed composite of graphite alkene；The above-mentioned foamed composite based on graphene oxide is placed in the hydrogen of mass fraction 15%
In iodic acid solution, flow back 2h at 100 DEG C, and the foamed composite based on redox graphene is obtained after being washed, being dried.
Repeated Compression 1000 times under 80% compression strain of obtained foamed composite, response rate are more than or equal to 95%, test it
Electromagnetic shielding performance, as shown in Fig. 2, its electromagnet shield effect is more than or equal to 44dB.
Embodiment 5
Neutral graphene oxide aqueous dispersions are freeze-dried, graphene oxide powder are obtained, by the oxygen of 100mg
The deionized water of 3.2g is added in graphite alkene powder, and one is placed in cell disruptor handles 20min under 60W power, obtains matter
Measure the graphene oxide aqueous dispersions of score 3%；Aperture polyimide foam is cut into the cubic block of 0.9g, is immersed in
In above-mentioned graphene oxide aqueous dispersions, repeatedly extruding polyimide foam makes graphene oxide aqueous dispersions uniform adsorption poly-
In the hole of acid imide foam, the mass ratio of the polyimide foam and graphene oxide is 9:1, is obtained after vacuum dried
Obtain the foamed composite based on graphene oxide；The above-mentioned foamed composite based on graphene oxide is placed in mass fraction
In 0.5% hydroiodic acid solution, flow back 3h at 90 DEG C, and the foam based on redox graphene is obtained after being washed, being dried
Composite material.Repeated Compression 1000 times under 80% compression strain of obtained foamed composite, response rate is more than or equal to
95%, its electromagnetic shielding performance is tested, as shown in Fig. 2, its electromagnet shield effect is more than or equal to 51dB.
Embodiment 6
Using the graphene oxide aqueous dispersions of commercially available mass fraction 3%；Open-celled polyurethane foam is cut into 0.9g
Cubic block, be immersed in above-mentioned graphene oxide aqueous dispersions, repeatedly extruding polyurethane foam makes graphene oxide water
Homogeneous dispersion is adsorbed in the hole of polyurethane foam, and the mass ratio of the polyurethane foam and graphene oxide is 9:1,
The foamed composite based on graphene oxide is obtained after vacuum dried；By the above-mentioned foam composite based on graphene oxide
Material is placed in the hydroiodic acid solution of mass fraction 40%, and flow back 3h at 100 DEG C, is obtained after being washed, being dried and is based on oxygen reduction
The foamed composite of graphite alkene.Repeated Compression 1000 times under 80% compression strain of obtained foamed composite are returned
Multiple rate is more than or equal to 95%, tests its electromagnetic shielding performance, as shown in Fig. 2, its electromagnet shield effect is more than or equal to 53dB.
Claims (3)
1. one kind has both electromagnetic wave shielding and flexible foamed composite, characterized in that graphene is in foam of polymers bone
One layer of three-dimensional continuous graphite alkene film is formed between frame and skeleton；
Have both electromagnetic shielding performance and flexible foamed composite be prepared by the following steps:
1) graphene oxide aqueous dispersions are freeze-dried, obtain graphene oxide powder, by graphene oxide powder plus
Enter deionized water, is placed in cell disruptor and handles 3~20min under 20~200W power, obtain mass fraction 0.05~3%
Graphene oxide aqueous dispersions；
2) foam of polymers is immersed in the graphene oxide aqueous dispersions that step 1) obtains, repeatedly extruding foam of polymers makes
Graphene oxide aqueous dispersions uniform adsorption will be adsorbed with the poly- of graphene oxide aqueous dispersions in the hole of foam of polymers
It closes object foam to dry in vacuum drying oven, obtains the foamed composite based on graphene oxide；
3) foamed composite based on graphene oxide is placed in the hydroiodic acid or mass fraction of mass fraction 0.5~40%
In 0.5~40% hydrazine hydrate solution, flow back 0.5~3h at 60~120 DEG C, obtains after being washed, being dried and is based on oxygen reduction
The foamed composite of graphite alkene；
The mass ratio of the foam of polymers and graphene oxide is 9~99:1.
2. the preparation method for having both electromagnetic shielding performance and flexible foamed composite of claim 1, it is characterized in that step
It is rapid as follows:
1) graphene oxide aqueous dispersions are freeze-dried, obtain graphene oxide powder, by graphene oxide powder plus
Enter deionized water, is placed in cell disruptor and handles 3~20min under 20~200W power, obtain mass fraction 0.05~3%
Graphene oxide aqueous dispersions；
2) foam of polymers is immersed in the graphene oxide aqueous dispersions that step 1) obtains, repeatedly extruding foam of polymers makes
Graphene oxide aqueous dispersions uniform adsorption will be adsorbed with the poly- of graphene oxide aqueous dispersions in the hole of foam of polymers
It closes object foam to dry in vacuum drying oven, obtains the foamed composite based on graphene oxide；
3) foamed composite based on graphene oxide is placed in the hydroiodic acid or mass fraction of mass fraction 0.5~40%
In 0.5~40% hydrazine hydrate solution, flow back 0.5~3h at 60~120 DEG C, obtains after being washed, being dried and is based on oxygen reduction
The foamed composite of graphite alkene；
The mass ratio of the foam of polymers and graphene oxide is 9~99:1.
3. method according to claim 2, it is characterized in that the foam of polymers is polyurethane foam, polyimide foam
Or the foam of polymers of silicon rubber foam aperture.
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