CN108329468A - A kind of preparation method of electromagnetic shielding composite material - Google Patents
A kind of preparation method of electromagnetic shielding composite material Download PDFInfo
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- CN108329468A CN108329468A CN201810105695.8A CN201810105695A CN108329468A CN 108329468 A CN108329468 A CN 108329468A CN 201810105695 A CN201810105695 A CN 201810105695A CN 108329468 A CN108329468 A CN 108329468A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0622—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0638—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with at least three nitrogen atoms in the ring
- C08G73/0644—Poly(1,3,5)triazines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0622—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0638—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with at least three nitrogen atoms in the ring
- C08G73/065—Preparatory processes
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation method of electromagnetic shielding composite material, this method includes：（1）Prepare hydridization graphene/carbon nano-tube dispersion liquid；（2）Prepare hydridization graphene and/or carbon nanotube and cyanate blended liquid；Cyanate is dissolved in acetone, with the step（1）After dispersion liquid obtained is mixed, continues 6~12 h of ultrasound and obtain finely dispersed dispersion liquid；（3）Remove solvent acetone；（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：120℃,0.5 h；160℃,0.5 h；180 DEG C, 2 h；190℃,2 h.The polymer matrix electromagnetic shielding composite material has the characteristics that shielding properties is adjustable, weight is close, preparation method is easy, of low cost and can be mass-produced.
Description
Technical field
The present invention relates to electro-magnetic screen function Material Fields, in particular to a kind of hydridization graphene/multi-wall carbon nano-tube
Pipe polymer matrix electromagnetic shielding composite material extremely preparation method.
Background technology
With the fast development of electronic information technology, electronic apparatus and telecommunication equipment are filled in aerospace, weapon
The military and civilians such as standby, mechanical equipment are widely used in field.Electromagnetic radiation has become dirty after water pollution, noise pollution, air
Another big pollution after dye, noxious waste pollution, in addition, with increasingly frequent, the space neck of people's space flight detected event
Complex environment in domain gradually attracts people's attention, electronics, proton and heavy charged particle irradiation, microgravity, elemental oxygen, space
The factors such as fragment and dust, vacuum charge and discharge, cold cycling, high-energy radiation constitute severe choose to the in-orbit military service of spacecraft
War.Currently, electro-magnetic screen layer generally use metallic conduction coating or sheet metal are covered on the component for needing to protect to come in fact with this
Existing shielding properties, but metal quality is big, increases equipment quality, especially in aerospace field, will produce expensive expense.This
Outside, there is also disadvantages perishable, oxidizable, not easy to be processed, easily cause precision instrument and the internal short-circuit of equipment, bring not
Necessary loss, seriously limit metal electromagnetic shielding field practical application.
Invention content
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, the primary purpose of the present invention is that providing a kind of miscellaneous
Graphite alkene/multi-walled carbon nanotube polymer matrix electromagnetic shielding composite material extremely preparation method.
The present invention adopts the following technical scheme that：
A kind of preparation method of electromagnetic shielding composite material, which is characterized in that the method includes：
（1）Prepare hydridization graphene/carbon nano-tube dispersion liquid
Graphene and/or multi-walled carbon nanotube and surfactant polyethylene or ethyl cellulose are added in acetone,
The ultrasonic disperse of 6~12 h is carried out to prepare hydridization graphene and/or carbon nano tube dispersion liquid；
（2）Prepare hydridization graphene and/or carbon nanotube and cyanate blended liquid
Cyanate is dissolved in acetone, with the step（1）After dispersion liquid obtained is mixed, continues 6~12 h of ultrasound and obtain
To finely dispersed dispersion liquid；
（3）Remove solvent acetone
The step is removed by the method for revolving（2）Solvent acetone in dispersion liquid obtained, and the slurry of acquisition is poured into
In mold, it is put into the degassing process for carrying out 0.5h~3h in vacuum drying oven under conditions of 80~100 DEG C；
（4）Curing molding
The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：120~140 DEG C,
0.5~1 h；160~180 DEG C, 0.5~1h；180~190 DEG C, 2~4 h；190~210 DEG C, 2~4 h.
According to above-mentioned preparation method, which is characterized in that the step（1）Middle addition is graphene and multi-wall carbon nano-tube
The mixture of pipe, and the mass ratio of graphene and multi-walled carbon nanotube is 1:1.
According to above-mentioned preparation method, which is characterized in that the step（1）The concentration of middle graphene and multi-walled carbon nanotube
For 2mg/mL, a concentration of 1mg/mL of surfactant polyethylene or ethyl cellulose.
Beneficial effects of the present invention：Nano material such as graphene and carbon nanotube have proved that its conduction is anti-through overtesting
Radianting capacity is splendid, not by external interference, has achieved the effect that radiation-proof anti-static, and conductive filler such as graphene or carbon are received
Mitron and cyanate carry out the compound polymer matrix composites for preparing enhancing and are expected to prepare a kind of light weight, low cost, anti-corruption
Erosion, while there is the shielding material of excellent absorbing property.
Description of the drawings
Fig. 1 is the capability of electromagnetic shielding curve of pure cyanate and cyanate nanocomposite.
Specific implementation mode
It elaborates below to the embodiment of the present invention, it is necessary to which indicated herein is that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, and the person skilled in the art in the field can be with
Some nonessential modifications and adaptations are made according to the content of aforementioned present invention.
The preparation method that the electromagnetic shielding of the present invention meets material includes the following steps：
（1）Prepare hydridization graphene/carbon nano-tube dispersion liquid
Graphene and/or multi-walled carbon nanotube and surfactant polyethylene or ethyl cellulose are added in acetone,
The ultrasonic disperse of 6~12 h is carried out to prepare hydridization graphene and/or carbon nano tube dispersion liquid；
（2）Prepare hydridization graphene and/or carbon nanotube and cyanate blended liquid
Cyanate is dissolved in acetone, with the step（1）After dispersion liquid obtained is mixed, continues ultrasound 6h~12 h and obtain
To finely dispersed dispersion liquid；
（3）Remove solvent acetone
The step is removed by the method for revolving（2）Solvent acetone in dispersion liquid obtained, and the slurry of acquisition is poured into
In mold, it is put into the degassing process for carrying out 0.5h~3h in vacuum drying oven under conditions of 80~100 DEG C；
（4）Curing molding
The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：120~140 DEG C,
0.5~1 h；160~180 DEG C, 0.5~1h；180~190 DEG C, 2~4 h；190~210 DEG C, 2~4 h.
Embodiment 1
（1）First a certain amount of graphene or multi-walled carbon nanotube are added in acetone, the concentration of graphene or multi-walled carbon nanotube
For 2mg/mL, a certain amount of surfactant polyethylene or ethyl cellulose, surfactant polyethylene or second are added
A concentration of 1mg/mL of base cellulose, carries out 12h supersound process, ultrasonic power 250W, and the graphene is liquid phase ultrasonic method
Prepared by stripping.
（2）A certain amount of cyanate is dissolved in acetone, it will（1）Middle dispersion liquid is added in cyanic acid ester solution and is simply stirred
6h is ultrasonically treated after mixing, the mass fraction that graphene or multi-walled carbon nanotube account for cyanate is 3%.
（3）Solvent acetone is removed by the method for revolving, slurry is poured into mold, is put into vacuum drying oven at 80 DEG C
Under conditions of carry out 0.5h degassing process.
（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：
120℃, 0.5h；160℃, 0.5h；180 DEG C, 2h；190℃, 2h.
Embodiment 2
（1）It is first 1 by mass ratio:1 graphene and multi-walled carbon nanotube is added in acetone, and a concentration of 2mg/mL is added
A certain amount of surfactant polyethylene, a concentration of 1mg/mL carry out 12h supersound process, ultrasonic power 250W.
（2）A certain amount of cyanate is dissolved in acetone, it will（1）Middle dispersion liquid is added in cyanic acid ester solution and is simply stirred
12h is ultrasonically treated after mixing, the mass fraction that graphene and multi-walled carbon nanotube account for cyanate altogether is 3%.
（3）Solvent acetone is removed by the method for revolving, slurry is poured into mold, is put into vacuum drying oven at 100 DEG C
Under conditions of carry out 1h degassing process.
（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：
120℃, 0.5h；160℃, 0.5h；180 DEG C, 2h；190℃, 2h.
Embodiment 3
（1）It is first 1 by mass ratio:1 graphene and multi-walled carbon nanotube is added in acetone, and a concentration of 1mg/mL is added
A certain amount of surfactant polyethylene or ethyl cellulose, a concentration of 2mg/mL carry out 12h supersound process, ultrasonic work(
Rate is 250W.
（2）A certain amount of cyanate is dissolved in acetone, it will（1）Middle dispersion liquid is added in cyanic acid ester solution and is simply stirred
12h is ultrasonically treated after mixing, the mass fraction that graphene and multi-walled carbon nanotube account for cyanate is 7%.
Solvent acetone is removed by the method for revolving, slurry is poured into mold, is put into vacuum drying oven at 100 DEG C
Under the conditions of carry out 2h degassing process.
（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：
120℃, 0.5h；160℃, 0.5h；180 DEG C, 2h；190℃, 2h.
Embodiment 4
（1）It is first 1 by mass ratio:1 graphene and multi-walled carbon nanotube is added in acetone, and a concentration of 1mg/mL is added
A certain amount of surfactant polyethylene or ethyl cellulose, a concentration of 2mg/mL carry out 6h supersound process, ultrasonic power
For 250W.
（2）A certain amount of cyanate is dissolved in acetone, it will（1）Middle dispersion liquid is added in cyanic acid ester solution and is simply stirred
6h is ultrasonically treated after mixing, the mass fraction that graphene and multi-walled carbon nanotube account for cyanate is 7%.
（3）Solvent acetone is removed by the method for revolving, slurry is poured into mold, is put into vacuum drying oven at 80 DEG C
Under conditions of carry out 2h degassing process.
（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：
120℃, 0.5h；160℃, 0.5h；180 DEG C, 2h；190℃, 2h.
Embodiment 5
（1）It is first 1 by mass ratio:1 graphene and multi-walled carbon nanotube is added in acetone, and a concentration of 1mg/mL is added
A certain amount of surfactant polyethylene or ethyl cellulose, a concentration of 2mg/mL carry out 6h supersound process, ultrasonic power
For 250W.
（2）A certain amount of cyanate is dissolved in acetone, it will（1）Middle dispersion liquid is added in cyanic acid ester solution and is simply stirred
12h is ultrasonically treated after mixing, the mass fraction that graphene and multi-walled carbon nanotube account for cyanate is 7%.
（3）Solvent acetone is removed by the method for revolving, slurry is poured into mold, is put into vacuum drying oven at 100 DEG C
Under conditions of carry out 3h degassing process.
（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：
120℃, 0.5h；160℃, 0.5h；180 DEG C, 2h；190℃, 2h.
Embodiment 6
（1）It is first 1 by mass ratio:1 graphene and multi-walled carbon nanotube is added in acetone, and a concentration of 1mg/mL is added
A certain amount of surfactant polyethylene or ethyl cellulose, a concentration of 2mg/mL carry out 12h supersound process, ultrasonic work(
Rate is 250W.
（2）A certain amount of cyanate is dissolved in acetone, it will（1）Middle dispersion liquid is added in cyanic acid ester solution and is simply stirred
6h is ultrasonically treated after mixing, the mass fraction that graphene and multi-walled carbon nanotube account for cyanate is 7%.
（3）Solvent acetone is removed by the method for revolving, slurry is poured into mold, is put into vacuum drying oven at 80 DEG C
Under conditions of carry out 3h degassing process.
（4）The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：
140℃, 1h；180℃, 1h；190 DEG C, 4h；210℃, 4h.
Fig. 1 is the capability of electromagnetic shielding curve of pure cyanate and cyanate nanocomposite, the number marked in figure
Represent the mass fraction of cyanate shared by conductive filler.The capability of electromagnetic shielding of straight polymer cyanate is very poor, conductive introducing
Capability of electromagnetic shielding is promoted after network, and in the case where adding equivalent filler, hydridization graphene/multi-walled carbon nanotube is conductive
The introducing of network than single filler conductive network to the promotion of the capability of electromagnetic shielding of polymer composites advantageously.
The hydridization graphene being prepared by the above method/multi-walled carbon nanotube polymer matrix is electromagnetically shielded composite wood
Material, it is characterized in that polymer matrix electromagnetic shielding material has graphene/multi-walled carbon nanotube hydridization conductive network, different dimensions
Conductive nano filler, which includes one-dimensional multi-walled carbon nanotube and two-dimensional graphene nanoscale twins, can cooperate with and effectively construct conductive network,
The polymer matrix is cyanate ester resin, and surfactant polyethylene or ethyl cellulose can not only improve hydridization conduction and fill out
Material dispersibility in the polymer, and can be between reinforcing filler and polymer interface interaction.The polymer matrix electromagnetism
Shielding composite has that shielding properties is adjustable, weight is close, preparation method is easy, the of low cost and spy that can be mass-produced
Point.
Claims (3)
1. a kind of preparation method of electromagnetic shielding composite material, which is characterized in that the method includes：
（1）Prepare hydridization graphene/carbon nano-tube dispersion liquid
Graphene and/or multi-walled carbon nanotube and surfactant polyethylene or ethyl cellulose are added in acetone,
The ultrasonic disperse of 6~12 h is carried out to prepare hydridization graphene and/or carbon nano tube dispersion liquid；
（2）Prepare hydridization graphene and/or carbon nanotube and cyanate blended liquid
Cyanate is dissolved in acetone, with the step（1）After dispersion liquid obtained is mixed, continues 6~12 h of ultrasound and obtain
To finely dispersed dispersion liquid；
（3）Remove solvent acetone
The step is removed by the method for revolving（2）Solvent acetone in dispersion liquid obtained, and the slurry of acquisition is poured into
In mold, it is put into the degassing process for carrying out 0.5h~3h in vacuum drying oven under conditions of 80~100 DEG C；
（4）Curing molding
The die horizontal for filling slurry is put into electric drying oven with forced convection, by following condition curing molding：120~140 DEG C,
0.5~1 h；160~180 DEG C, 0.5~1h；180~190 DEG C, 2~4 h；190~210 DEG C, 2~4 h.
2. preparation method according to claim 1, which is characterized in that the step（1）Middle addition is graphene and more
The mixture of wall carbon nano tube, and the mass ratio of graphene and multi-walled carbon nanotube is 1:1.
3. preparation method according to claim 1 or 2, which is characterized in that the step（1）Middle graphene and multi wall carbon are received
A concentration of 1mg/mL of a concentration of 2mg/mL of mitron, surfactant polyethylene or ethyl cellulose.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591579A (en) * | 2019-08-13 | 2019-12-20 | 深圳烯湾科技有限公司 | Electromagnetic shielding heat dissipation film and preparation method and application thereof |
| CN111234526A (en) * | 2020-03-03 | 2020-06-05 | 西安理工大学 | Preparation method of coffee grounds/graphene/cyanate ester composite material |
| CN111269570A (en) * | 2020-03-24 | 2020-06-12 | 西安理工大学 | Preparation method of carbonized towel gourd/graphene-carbon nanotube composite material |
| CN112851986A (en) * | 2021-03-19 | 2021-05-28 | 北京理工大学 | Flexible wave-absorbing composite material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591579A (en) * | 2019-08-13 | 2019-12-20 | 深圳烯湾科技有限公司 | Electromagnetic shielding heat dissipation film and preparation method and application thereof |
| CN110591579B (en) * | 2019-08-13 | 2021-08-31 | 深圳烯湾科技有限公司 | Electromagnetic shielding heat dissipation film and preparation method and application thereof |
| CN111234526A (en) * | 2020-03-03 | 2020-06-05 | 西安理工大学 | Preparation method of coffee grounds/graphene/cyanate ester composite material |
| CN111234526B (en) * | 2020-03-03 | 2022-07-29 | 西安昊友航天复合材料有限公司 | Preparation method of coffee grounds/graphene/cyanate ester composite material |
| CN111269570A (en) * | 2020-03-24 | 2020-06-12 | 西安理工大学 | Preparation method of carbonized towel gourd/graphene-carbon nanotube composite material |
| CN111269570B (en) * | 2020-03-24 | 2022-07-29 | 西安昊友航天复合材料有限公司 | Preparation method of carbonized towel gourd/graphene-carbon nanotube composite material |
| CN112851986A (en) * | 2021-03-19 | 2021-05-28 | 北京理工大学 | Flexible wave-absorbing composite material and preparation method thereof |
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Application publication date: 20180727 |