CN110418560A - A kind of graphene-based electromagnetic shielding adhesive tape and preparation method thereof - Google Patents
A kind of graphene-based electromagnetic shielding adhesive tape and preparation method thereof Download PDFInfo
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- CN110418560A CN110418560A CN201910496969.5A CN201910496969A CN110418560A CN 110418560 A CN110418560 A CN 110418560A CN 201910496969 A CN201910496969 A CN 201910496969A CN 110418560 A CN110418560 A CN 110418560A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The present invention provides a kind of graphene-based electromagnetic shielding adhesive tape and preparation method thereof, is that graphene oxide solution is placed in the syringe of electrostatic atomizer, using copper foil as receiver, making alive, and move in parallel receiver, electrostatic spray, obtain the modified copper foil of graphene oxide；The modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction obtains the modified copper foil of graphene layer；Powdered graphite is added in polymer solution, ball milling decentralized processing, low-speed centrifugal removal precipitating, high speed centrifugation takes out supernatant, obtains graphene polymer dispersion liquid；After the graphene coated polymer dispersion liquid in conducting PET surface, baking and curing, it is coated with conductive pressure sensitive adhesive, baking and curing, obtains graphene-based two-sided conductive tape again；The copper foil that two-sided conductive tape and graphene layer are modified successively alternately is covered on conducting PET surface, repeats alternately to cover, finally with two-sided conductive tape and PET release film pressurizing attaching, obtains graphene-based electromagnetic shielding adhesive tape.
Description
Technical field
The invention belongs to electromagnetic shielding adhesive tape technical fields, and in particular to a kind of graphene-based electromagnetic shielding adhesive tape and its system
Preparation Method.
Background technique
The 5G epoch gradually close on, it is high-frequency introduce, the upgrading of hardware components and networked devices and antenna amount
It is doubled and redoubled, between equipment and equipment and the electromagnetic interference of equipment inside itself is ubiquitous, electromagnetic interference and electromagnetic radiation pair
The harm of electronic equipment is also got worse.The update of simultaneous electronic product upgrades, and the power consumption of equipment constantly increases, future
The bottleneck of high-frequency high power electronic product first is that its generate electromagnetic radiation, in order to solve this problem, electronic product is being set
More and more electromagnetic shielding devices will be added in timing.Therefore the effect of electromagnetic shielding and device needs ever more important, future
It asks sustainable growth also.
Electromagnetic shielding device is that secondary development is carried out on the basis of electromagnetic shielding material, and required material must have good
Good electric conductivity.According to the addition manner of conductive filler, electromagnetic shielding material can be divided into metal class, filling class and surface cladding layer and
Conductive coating class, wherein filling class be added in nonconducting substrate such as silica gel, plastics a certain proportion of conductive filler to
So that materials conductive, conductive filler can be the materials such as sheet metal, metal powder, wire, metallic fiber or metalized fibers,
Surface cladding layer and conductive coating class are that the substrates such as conductive fabric are electroplated.
Currently, electromagnetic shielding adhesive tape is a kind of to integrate metal class, filling class and surface cladding layer and conductive coating class
Light and thin type electromagnetic shielding material has good Research Prospects.A kind of electromagnetism wave screen disclosed in Chinese patent CN106700961A
Film and the highly transparent strong electromagnetic wave shielding tape based on it are covered, by silver nanowires, PEDOT:PSS, graphene, water soluble acrylic acid
Resin, waterborne polyurethane resin, curing agent, small molecule dispersing agent, levelling agent, defoaming agent and water are mixed in proportion, are obtained electric
Magnetic wave shields slurry, then electromagnetic wave shielding slurry is coated on to the one side of transparent substrates by coating machine, then heating, drying,
Electromagnetic shielding film is formed, binder is coated on to the another side of transparent substrates by coating machine, formation adhesive layer finally will be from
Type paper and adhesive layer roll-forming, then cutting cuts to get highly transparent strong electromagnetic wave shielding tape is arrived.This method preparation
Under the premise of silver-colored dosage is effectively reduced in electromagnetic shielding adhesive tape, the transmitance and shield effectiveness of electromagnetic shielding film are improved.Therefore,
How on the basis of guaranteeing that electromagnetic wave shielding adhesive tape is frivolous, the shield effectiveness of electromagnetic wave shielding adhesive tape is improved, is had extensive
Research Prospects.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of graphene-based electromagnetic shielding adhesive tapes and preparation method thereof, by stone
Black alkene is used as metal conducting layer after copper foil surface forms stable layered distribution, replaces attachment with graphene-based two-sided conductive tape
In release film surface, electric conductivity and the excellent graphene-based electromagnetic shielding adhesive tape of machining property is prepared in pressurizing attaching.
In order to solve the above technical problems, the technical scheme is that
A kind of graphene-based electromagnetic shielding adhesive tape, the graphene-based electromagnetic shielding adhesive tape includes release film, graphene-based
The copper foil that two-sided conductive tape and graphene layer are modified, at least two layers of quantity of the modified copper foil of the graphene layer, the stone
At least three layers of the quantity of the two-sided conductive tape of mertenyl.
As a preferred embodiment of the above technical solution, the conducting PET film is that metallic nickel or nickel alloy micrometer/nanometer particle adulterate
Homogeneous conductive film.
A kind of preparation method of graphene-based electromagnetic shielding adhesive tape of the present invention, comprising the following steps:
(1) graphene oxide solution is placed in the syringe of electrostatic atomizer, using copper foil as receiver, making alive,
And move in parallel receiver, electrostatic spray, obtain the modified copper foil of graphene oxide；
(2) the modified copper foil of the graphene oxide of step (1) preparation is placed under hydrogen environment, heating reduction obtains stone
The modified copper foil of black alkene layer；
(3) powdered graphite is added in polymer solution, ball milling, ultrasonic disperse processing, low-speed centrifugal removal precipitating is high
Supernatant is taken out in speed centrifugation, obtains graphene polymer dispersion liquid；
(4) after the graphene polymer dispersion liquid of conducting PET surface coating step (3) preparation, baking and curing, re-coating
Conductive pressure sensitive adhesive, baking and curing, obtains graphene-based two-sided conductive tape again；
(5) conducting PET surface successively alternately covering step (4) preparation two-sided conductive tape and step (2) preparation
The modified copper foil of graphene layer repeats alternately to cover, the two-sided conductive tape and PET release film of last covering step (4) preparation,
Pressurizing attaching obtains graphene-based electromagnetic shielding adhesive tape.
As a preferred embodiment of the above technical solution, in the step (1), the content of graphene oxide solution is 20-25mg/
mL。
As a preferred embodiment of the above technical solution, in the step (1), the voltage of electrostatic spray is 5-8KV, receives distance and is
10-15cm, the rate 0.5-0.8cm/s that receiver moves in parallel.
As a preferred embodiment of the above technical solution, in the step (2), the temperature for heating reduction is 500-600 DEG C, and the time is
4-6h。
As a preferred embodiment of the above technical solution, in the step (2), the number of plies of graphene in the modified copper foil of graphene layer
It is 8-15 layers.
As a preferred embodiment of the above technical solution, in the step (3), in graphene polymer dispersion liquid graphene with polymerize
The mass ratio of object is 1:8-10.
As a preferred embodiment of the above technical solution, in the step (3), the revolving speed of low-speed centrifugal is 500-800r/min, high
The revolving speed of speed centrifugation is 2000-2500r/min.
As a preferred embodiment of the above technical solution, in the step (4), graphene contains in graphene-based two-sided conductive tape
Amount is 3-5wt%.
Compared with prior art, the invention has the following advantages:
Contain conducting PET film, two-sided conductive tape and graphene in graphene-based electromagnetic shielding adhesive tape prepared by the present invention
The modified copper foil of layer, wherein conducting PET film is the homogeneous conductive film that metallic nickel or nickel alloy micrometer/nanometer particle adulterate, conductive
The electric conductivity of PET film is excellent, then by being alternately arranged two-sided conductive tape and graphene layer modification in conducting PET film surface
Copper foil, make electromagnetic shielding adhesive tape realization protect layer by layer, be remarkably improved the effectiveness of electromagnetic shielding adhesive tape, furthermore this
Invention is modified place to two-sided conductive tape and copper foil using graphene on the basis of guaranteeing that electromagnetic shielding adhesive tape is frivolous
Reason, graphene form frivolous graphene sheet layer on the surface of copper foil using electrostatic inkjet technology, and by making copper foil receiver
Translation rate be greater than graphene solution drop rate, keep the arrangement mode of the graphene sheet layer of copper foil surface regular, stone
The electric conductivity of the modified copper foil of black alkene layer significantly improves, flexibility more preferably, in addition, being also added to graphene as conductive filler
In two-sided conductive tape, makes that also there is the conductive filler being distributed in the form of sheets in two-sided conductive tape, have later by pressurizing attaching
Conducive to the tightness combined between the copper foil that two-sided conductive tape and graphene layer are modified is improved, be conducive to further increase graphite
The effectiveness and mechanical performance of alkenyl electromagnetic shielding adhesive tape.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
(1) graphene oxide solution of 20mg/mL is placed in the syringe of electrostatic atomizer, is to receive with copper foil
Device, making alive, and receiver is moved in parallel according to the rate of 0.5cm/s, under the voltage of 5KV, receiving distance is 10cm, quiet
Electron spray 5min obtains the modified copper foil of graphene oxide.
(2) the modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction 4h, obtains graphite at 500 DEG C
The modified copper foil of alkene layer, wherein the number of plies of graphene is 8 layers in the modified copper foil of graphene layer.
(3) powdered graphite is added in polymer solution, is 10:1, ball milling decentralized processing 90min according to ball milling ratio, surpasses
Sound dispersion, the low-speed centrifugal removal precipitating under the revolving speed of 500r/min, high speed centrifugation takes out supernatant under the revolving speed of 2000r/min
Liquid obtains graphene polymer dispersion liquid, and wherein the mass ratio of graphene and polymer is 1 in graphene polymer dispersion liquid:
8。
(4) the homogeneous graphene coated polymerization of conducting PET film surface adulterated in metallic nickel or nickel alloy micrometer/nanometer particle
Object dispersion liquid, the baking and curing 10min at 50 DEG C are coated with conductive pressure sensitive adhesive, and the baking and curing at 50 DEG C, obtains graphite again
The two-sided conductive tape of alkenyl, wherein the content of graphene is 3wt% in graphene-based two-sided conductive tape.
(5) metal nickel nano particle doping homogeneous conducting PET film surface successively alternately cover two-sided conductive tape and
The modified copper foil of graphene layer repeats alternately covering 2 times, last two-sided conductive tape and PET release film, patch of pressurizeing at 5MPa
3min is closed, graphene-based electromagnetic shielding adhesive tape is obtained.
Embodiment 2:
(1) graphene oxide solution of 25mg/mL is placed in the syringe of electrostatic atomizer, is to receive with copper foil
Device, making alive, and receiver is moved in parallel according to the rate of 0.8cm/s, under the voltage of 8KV, receiving distance is 15cm, quiet
Electron spray 30min obtains the modified copper foil of graphene oxide.
(2) the modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction 6h, obtains graphite at 600 DEG C
The modified copper foil of alkene layer, wherein the number of plies of graphene is 15 layers in the modified copper foil of graphene layer.
(3) powdered graphite is added in polymer solution, according to ball milling ratio be 10:1, ball milling decentralized processing 120min,
Ultrasonic disperse, the low-speed centrifugal removal precipitating under the revolving speed of 800r/min, under the revolving speed of 2500r/min in high speed centrifugation taking-up
Clear liquid obtains graphene polymer dispersion liquid, and wherein the mass ratio of graphene and polymer is in graphene polymer dispersion liquid
1:10。
(4) the homogeneous graphene coated polymerization of conducting PET film surface adulterated in metallic nickel or nickel alloy micrometer/nanometer particle
Object dispersion liquid, the baking and curing 10min at 60 DEG C are coated with conductive pressure sensitive adhesive, and the baking and curing at 60 DEG C, obtains graphite again
The two-sided conductive tape of alkenyl, wherein the content of graphene is 5wt% in graphene-based two-sided conductive tape.
(5) nickel alloy micro particles doping homogeneous conducting PET film surface successively alternately cover two-sided conductive tape and
The modified copper foil of graphene layer repeats alternately covering 5 times, last two-sided conductive tape and PET release film, patch of pressurizeing at 7MPa
5min is closed, graphene-based electromagnetic shielding adhesive tape is obtained.
Embodiment 3:
(1) graphene oxide solution of 23mg/mL is placed in the syringe of electrostatic atomizer, is to receive with copper foil
Device, making alive, and receiver is moved in parallel according to the rate of 0.6cm/s, under the voltage of 7KV, receiving distance is 12cm, quiet
Electron spray 10min obtains the modified copper foil of graphene oxide.
(2) the modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction 5h, obtains graphite at 550 DEG C
The modified copper foil of alkene layer, wherein the number of plies of graphene is 12 layers in the modified copper foil of graphene layer.
(3) powdered graphite is added in polymer solution, according to ball milling ratio be 10:1, ball milling decentralized processing 100min,
Ultrasonic disperse, the low-speed centrifugal removal precipitating under the revolving speed of 600r/min, under the revolving speed of 2300r/min in high speed centrifugation taking-up
Clear liquid obtains graphene polymer dispersion liquid, and wherein the mass ratio of graphene and polymer is in graphene polymer dispersion liquid
1:9。
(4) the homogeneous graphene coated polymerization of conducting PET film surface adulterated in metallic nickel or nickel alloy micrometer/nanometer particle
Object dispersion liquid, the baking and curing 10min at 55 DEG C are coated with conductive pressure sensitive adhesive, and the baking and curing at 53 DEG C, obtains graphite again
The two-sided conductive tape of alkenyl, wherein the content of graphene is 4.5wt% in graphene-based two-sided conductive tape.
(5) the homogeneous conducting PET film surface of nickel alloy nanoparticle doped successively alternately cover two-sided conductive tape and
The modified copper foil of graphene layer repeats alternately covering 3 times, last two-sided conductive tape and PET release film, patch of pressurizeing at 6MPa
4min is closed, graphene-based electromagnetic shielding adhesive tape is obtained.
Embodiment 4:
(1) graphene oxide solution of 21mg/mL is placed in the syringe of electrostatic atomizer, is to receive with copper foil
Device, making alive, and receiver is moved in parallel according to the rate of 0.6cm/s, under the voltage of 7KV, receiving distance is 12cm, quiet
Electron spray 25min obtains the modified copper foil of graphene oxide.
(2) the modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction 5.5h, obtains graphite at 55 DEG C
The modified copper foil of alkene layer, wherein the number of plies of graphene is 12 layers in the modified copper foil of graphene layer.
(3) powdered graphite is added in polymer solution, according to ball milling ratio be 10:1, ball milling decentralized processing 110min,
Ultrasonic disperse, the low-speed centrifugal removal precipitating under the revolving speed of 750r/min, under the revolving speed of 2150r/min in high speed centrifugation taking-up
Clear liquid obtains graphene polymer dispersion liquid, and wherein the mass ratio of graphene and polymer is in graphene polymer dispersion liquid
1:9.5。
(4) the homogeneous graphene coated polymerization of conducting PET film surface adulterated in metallic nickel or nickel alloy micrometer/nanometer particle
Object dispersion liquid, the baking and curing 10min at 55 DEG C are coated with conductive pressure sensitive adhesive, and the baking and curing at 57 DEG C, obtains graphite again
The two-sided conductive tape of alkenyl, wherein the content of graphene is 4.2wt% in graphene-based two-sided conductive tape.
(5) metal nickel nano particle doping homogeneous conducting PET film surface successively alternately cover two-sided conductive tape and
The modified copper foil of graphene layer repeats alternately covering 4 times, last two-sided conductive tape and PET release film, patch of pressurizeing at 7MPa
3min is closed, graphene-based electromagnetic shielding adhesive tape is obtained.
Embodiment 5:
(1) graphene oxide solution of 20mg/mL is placed in the syringe of electrostatic atomizer, is to receive with copper foil
Device, making alive, and receiver is moved in parallel according to the rate of 0.8cm/s, under the voltage of 5KV, receiving distance is 15cm, quiet
Electron spray 5min obtains the modified copper foil of graphene oxide.
(2) the modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction 4h, obtains graphite at 600 DEG C
The modified copper foil of alkene layer, wherein the number of plies of graphene is 15 layers in the modified copper foil of graphene layer.
(3) powdered graphite is added in polymer solution, is 10:1, ball milling decentralized processing 90min according to ball milling ratio, surpasses
Sound dispersion, the low-speed centrifugal removal precipitating under the revolving speed of 800r/min, high speed centrifugation takes out supernatant under the revolving speed of 2000r/min
Liquid obtains graphene polymer dispersion liquid, and wherein the mass ratio of graphene and polymer is 1 in graphene polymer dispersion liquid:
10。
(4) the homogeneous graphene coated polymerization of conducting PET film surface adulterated in metallic nickel or nickel alloy micrometer/nanometer particle
Object dispersion liquid, the baking and curing 10min at 50 DEG C are coated with conductive pressure sensitive adhesive, and the baking and curing at 60 DEG C, obtains graphite again
The two-sided conductive tape of alkenyl, wherein the content of graphene is 3wt% in graphene-based two-sided conductive tape.
(5) nickel alloy micro particles doping homogeneous conducting PET film surface successively alternately cover two-sided conductive tape and
The modified copper foil of graphene layer repeats alternately covering 5 times, last two-sided conductive tape and PET release film, patch of pressurizeing at 5MPa
5min is closed, graphene-based electromagnetic shielding adhesive tape is obtained.
Embodiment 6:
(1) graphene oxide solution of 25mg/mL is placed in the syringe of electrostatic atomizer, is to receive with copper foil
Device, making alive, and receiver is moved in parallel according to the rate of 0.5cm/s, under the voltage of 8KV, receiving distance is 10cm, quiet
Electron spray 30min obtains the modified copper foil of graphene oxide.
(2) the modified copper foil of graphene oxide is placed under hydrogen environment, heating reduction 6h, obtains graphite at 500 DEG C
The modified copper foil of alkene layer, wherein the number of plies of graphene is 11 layers in the modified copper foil of graphene layer.
(3) powdered graphite is added in polymer solution, according to ball milling ratio be 10:1, ball milling decentralized processing 120min,
Ultrasonic disperse, the low-speed centrifugal removal precipitating under the revolving speed of 500r/min, under the revolving speed of 2500r/min in high speed centrifugation taking-up
Clear liquid obtains graphene polymer dispersion liquid, and wherein the mass ratio of graphene and polymer is in graphene polymer dispersion liquid
1:8。
(4) the homogeneous graphene coated polymerization of conducting PET film surface adulterated in metallic nickel or nickel alloy micrometer/nanometer particle
Object dispersion liquid, the baking and curing 10min at 60 DEG C are coated with conductive pressure sensitive adhesive, and the baking and curing at 50 DEG C, obtains graphite again
The two-sided conductive tape of alkenyl, wherein the content of graphene is 3.9wt% in graphene-based two-sided conductive tape.
(5) metallic nickel micro particles doping homogeneous conducting PET film surface successively alternately cover two-sided conductive tape and
The modified copper foil of graphene layer repeats alternately covering 4 times, last two-sided conductive tape and PET release film, pressurizes at 6.5MPa
It is bonded 4min, obtains graphene-based electromagnetic shielding adhesive tape.
Through detecting, the graphene-based electromagnetic shielding adhesive tape and comparative example (CN106700961A) of embodiment 1-6 preparation are open
Transparent strong electromagnetic wave shielding tape electromagnetic shielding performance and mechanical performance result it is as follows:
As seen from the above table, the effectiveness of graphene-based electromagnetic shielding adhesive tape prepared by the present invention is more excellent, and
More preferably, using effect is more preferable for flexibility.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (10)
1. a kind of graphene-based electromagnetic shielding adhesive tape, it is characterised in that: the graphene-based electromagnetic shielding adhesive tape includes conducting PET
The modified copper foil of film, graphene-based two-sided conductive tape and graphene layer, the quantity of the modified copper foil of the graphene layer is at least
Two layers, at least three layers of the quantity of the graphene-based two-sided conductive tape.
2. a kind of graphene-based electromagnetic shielding adhesive tape according to claim 1, which is characterized in that the conducting PET film is
Metallic nickel or the homogeneous conductive film of nickel alloy micrometer/nanometer particle doping.
3. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape described in claims 1 or 2, which is characterized in that including
Following steps:
(1) graphene oxide solution is placed in the syringe of electrostatic atomizer, using copper foil as receiver, making alive, and will
Receiver moves in parallel, electrostatic spray, obtains the modified copper foil of graphene oxide；
(2) the modified copper foil of the graphene oxide of step (1) preparation is placed under hydrogen environment, heating reduction obtains graphene
The modified copper foil of layer；
(3) powdered graphite is added in polymer solution, ball milling, ultrasonic disperse processing, low-speed centrifugal removal precipitating, at a high speed from
The heart takes out supernatant, obtains graphene polymer dispersion liquid；
(4) after the graphene polymer dispersion liquid of conducting PET surface coating step (3) preparation, baking and curing, re-coating is conductive
Pressure sensitive adhesive, baking and curing, obtains graphene-based two-sided conductive tape again；
(5) in the conducting PET surface graphite that successively alternately prepared by the two-sided conductive tape of covering step (4) preparation and step (2)
The modified copper foil of alkene layer repeats alternately to cover, the two-sided conductive tape and PET release film of last covering step (4) preparation, pressurization
Fitting, obtains graphene-based electromagnetic shielding adhesive tape.
4. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: the step
Suddenly in (1), the content of graphene oxide solution is 20-25mg/mL.
5. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: the step
Suddenly in (1), the voltage of electrostatic spray is 5-8KV, and receiving distance is 10-15cm, the rate 0.5- that receiver moves in parallel
0.8cm/s。
6. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: the step
Suddenly in (2), the temperature for heating reduction is 500-600 DEG C, time 4-6h.
7. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: the step
Suddenly in (2), the number of plies of graphene is 8-15 layers in the modified copper foil of graphene layer.
8. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: the step
Suddenly in (3), the mass ratio of graphene and polymer is 1:8-10 in graphene polymer dispersion liquid.
9. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: the step
Suddenly in (3), the revolving speed of low-speed centrifugal is 500-800r/min, and ultracentrifugal revolving speed is 2000-2500r/min.
10. a kind of preparation method of graphene-based electromagnetic shielding adhesive tape according to claim 3, it is characterised in that: described
In step (4), the content of graphene is 3-5wt% in graphene-based two-sided conductive tape.
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