CN109553793A - A kind of flexibility PA graphene electromagnetic shielding material and preparation method thereof - Google Patents
A kind of flexibility PA graphene electromagnetic shielding material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to technical field of electromagnetic shielding, especially a kind of flexibility PA graphene electromagnetic shielding material and preparation method thereof.The preparation method includes carrying out sided corona treatment to flexible PA film, preparing viscous paste, blade coating viscous paste, drying and other steps.Water-based acrylic resin is used in preparation method as bonding agent.Compared with prior art, the present invention prepares the simple process of electromagnetic shielding material, and process environmental protection, uniformly, obtained finished product has many advantages, such as Soft, foldable to blade coating, and electromagnetic shielding performance is excellent, wide market.
Description
Technical field
The present invention relates to electromagnetic shielding material, be particularly based on flexible electromagnetic shielding material of graphene and preparation method thereof and
Using.
Background technique
With information technology, the development of electronics industry, electronics and IT products are applied in all trades and professions, are seen everywhere.Promoting
Into while economical, society is fast-developing, the electromagnetic pollution got worse is also brought.In order to avoid electromagenetic wave radiation is to electronics
The interference of electric product improves the stability that electronic and electrical equipment uses, accuracy.In addition to need to correctly design circuit and reasonable cloth
Outside office's electronic component, implementing anti-radiation protection to it using electromagnetic shielding material is effective method.
Electromagnetic shielding, i.e., enter electromagnetic energy caused by electromagnetic radiation field source not using the reflection of shield, decaying etc.
By shielding area.In general, shield effectiveness shield effectiveness SE (Shielding of the shielding material to space point
Effectiveness it) indicates, i.e. wherein, field strength when E0 is no shielding material, E is that have shield to SE=20lg (E0/E)
The field strength afterwards.
When Electromagnetic Wave Propagation reaches shielding material surface, is usually decayed by 3 kinds of different mechanisms (referring to Fig. 1): 1. being existed
The reflection loss of incidence surface;2. the loss that the electromagnetic wave for entering shield not by reflection is absorbed by material;3. in shield
Internal multiple reflections loss.
Electromagnetic wave can be calculated as follows by the total shield effectiveness of shielding material: wherein, SE is electromagnetic shielding effect to SE=A+R+B
Fruit, R are the decaying of surface individual reflection, and A is absorption loss, and B is multiple reflection inside loss.
1) reflection loss reflection loss is due to caused by mismatching between space impedance and the intrinsic resistance of shielded layer.Tool
There is the material of higher conductivity or more low magnetic permeability, reflection loss is bigger, and reflection loss not only has with the impedance of material surface
Close distance dependent of the also with the type of radiation source and shield to radiation source.
2) absorption loss is electric dipole in conductor material or magnetic dipole and electromagnetic field effect as a result, due to absorbing
A is lost to occur in shielding material, it is unrelated with type (electric field wave or the magnetic field wave) of wave, with the thickness of shielded layer, frequency,
Conductivity and magnetic conductivity are related.The thickness of material increases, and A value is also bigger.
3) multipath reflection is lost.After passing through attenuated inside due to transmitted wave, and the other side of shielded layer is encountered, in this side
Face is reflected and is transmitted again, and back wave is so reflected repeatedly again by inside, energy is made to decay rapidly.
Electromagnetic shielding material is mostly composite material and the silver system, copper of metal plate, wire mesh, metal and plastics at present
There are also flexible electromagnetic shielding material-metallized textiles for the electromagnetism coating of the types such as system, nickel system.These electromagnetic shielding materials are resistance to
It is not good enough in corrosivity, and complex manufacturing technology, manufacturing process not environmentally, need to contact volatile acid and heavy metal.
Graphene (Graphene) is that carbon atom is formed with sp2 hybridized orbit, has planar hexangle type honeycomb
The material of lattice.Graphene is a kind of nano material with good chemical stability, excellent electric conductivity.
PA film has wear-resisting, tough, drug-resistant, heat-resisting, cold-resistant, easily molded, self-lubricating, nothing compared with general plastics
The advantages that poison, easy dyeing, and the feature of film maximum is that OTR oxygen transmission rate is low.
Summary of the invention
It is an object of the invention to overcome defect existing in the prior art, a kind of flexibility PA graphene electromagnetic shielding is provided
Material and preparation method thereof.The shielding material has excellent flexibility, shield effectiveness, Corrosion Protection, acidproof, alkaline-resisting, simultaneously
Preparation method also has many advantages, such as that simple process, process are environmentally protective.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) first that the processing of PA film surface is clean, using sided corona treatment appropriate, film surface forms tiny poroid, reaches
To certain roughness, increase the adhesive strength of subsequent film;
It (2) is (0.9~1.1): (0.9~1.2): water-based acrylic resin, the stone of (0.005~0.008) by mass ratio
Black alkene slurry, defoaming agent are added in vacuum mixer, and adjustings negative pressure is -0.04mpa~-0.06mpa, revolving speed for 1200~
1800r/min, stirring duration 12~for 24 hours;
(3) it is calculated according to graphene stock quality, weighs 4.5%~5.5% polyether modified siloxane levelling agent addition
In the slurry obtained to step (2), adjusting negative pressure is -0.04mpa~-0.06mpa, and revolving speed is 200~600r/min, when stirring
Long 1.5~3h;
(4) slurry for obtaining step (3) takes out, smooth, uniformly scratches the PA crossed in the sided corona treatment that step (1) obtains
On film, with a thickness of 0.4~0.8mm, graphene coating film is formed in the PA film surface that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven to get flexibility PA graphene electromagnetic shielding material is arrived.
Preferably, the PA film prepared in the step (1) with a thickness of 0.02~0.4mm.
Preferably, drying temperature is 40~55 DEG C in the step (5), and drying time is 1.5~3h;More preferably, it does
Dry temperature is 45 DEG C, drying time 2h.
Preferably, the graphene slurry in the step (2) includes graphene, water and dispersing agent, the graphene, water
And the mass ratio of dispersing agent is (25~35): (64~73): (1~2);More preferably, the graphene, water and dispersing agent
Mass ratio be 30:69:1.Preferably, the dispersing agent is the Silok-7170W type dispersing agent that Si Luoke China provides.
Preferably, the polyether modified siloxane levelling agent in the step (3) is GSK-550 polyether modified siloxane levelling
Agent is produced by Dongguan City Gauss into Fine Chemical Co., Ltd, and usage amount is the 5% of graphene stock quality.
Preferably, the defoaming agent in the step (2) is DQ-2209 defoaming agent, by Dongguan City a century grand plan chemical science and technology
Co., Ltd's production;
Preferably, PA film surface is completely handled in the step (1), is to use to have soaked ethanol solution
The method of non-dust cloth wiping.
Preferably, a kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) first that the processing of 0.2mm thickness PA film surface is clean, using sided corona treatment appropriate, film surface forms tiny
It is poroid, reach certain roughness, increases the adhesive strength of subsequent film;
(2) water-based acrylic resin, graphene slurry, defoaming agent that mass ratio is 1:1:0.005 are added and are stirred under vacuum
In device, adjusting negative pressure is -0.05mpa, revolving speed 1600r/min, stirs duration 12h;
(3) it is calculated according to graphene stock quality, the polyether modified siloxane levelling agent for weighing 5% is added to step (2)
In obtained slurry, adjusting negative pressure is -0.05mpa, revolving speed 400r/min, stirs duration 2h;
(4) slurry for obtaining step (3) takes out, smooth, uniformly scratches the PA crossed in the sided corona treatment that step (1) obtains
On film, with a thickness of 0.4mm, graphene coating film is formed in the PA film surface that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven, drying temperature is 45 DEG C, drying time be 2h to get
To flexible PA graphene electromagnetic shielding material.
Obtained flexible PA graphene electromagnetic shielding material is subjected to aging process, is placed on aging in air drying environment
24h.Then its electromagnet shield effect is tested.In 300KHZ~1.5GHZ band limits, electromagnetic shielding effectiveness is more than or equal to
36dB has excellent shield effectiveness.
In addition, the application the invention further relates to the resulting finished product of above-mentioned preparation method in electromagnetic shielding field.
Compared with prior art, the advantages and beneficial effects of the present invention are:
(1) flexibility PA film graphene electromagnetic shielding material is as electromagnetic shielding film in the present invention, only with graphite when preparation
The conventional samples such as alkene slurry and water-based acrylic resin, defoaming agent, reagent, and use de-airing mixer, doctor knife coater, dryer
Equal conventional equipments, have the characteristics that manufacture craft is simple and environmentally-friendly, low in cost.
It (2) the use of medicament and raw material is all innocuous substance in the present invention, preparation process is environmentally protective.
(3) flexibility PA graphene coating film prepared by the present invention has superior barrier efficiency, Corrosion Protection, acidproof, resistance to
Alkali.And due to being flexible material, usage scenario is more extensive.Graphene flexible electromagnetic shielding film, thickness made of the present invention
Only 0.1~1.2mm, it is bent, distort, tear open and be cut into various shape, use scope is wide.
(4) present invention uses water-based acrylic resin as bonding agent, that is, enhances adhesive strength, and be good for the environment.
Traditional resin is usually all that in the construction process and in solidification process, will discharge largely organic wave using organic solvent
Object is sent out, causes the pollution of atmosphere, environment, or even cause harm to the human body.
(5) present invention is dried the semi-finished product after blade coating using suitable temperature, controls rate of drying, keeps away
The phenomenon that cavity occurs in graphene film layer is exempted from.
(6) water-based acrylic resin that the present invention uses is the main matter for scratching the film-forming after PA substrate surface,
Graphene is filled wherein as conductive materials, and forms conductive network.Water-based acrylic resin can be shunk in solidification, so that
It is close to each other to fill graphene therein, and contacts, is more likely formed conductive channel, this synergistic effect, enhance finally at
The electric conductivity of product also improves conductive stability.
(7) present invention has widened the purposes of graphene, improves the practical application value of graphene to a certain extent.
Detailed description of the invention
Fig. 1 is principle of electromagnetic shield-ing schematic diagram.
Fig. 2 is the structural schematic diagram that flexibility PA graphene is electromagnetically shielded membrane material.
Fig. 3 a is the graphene coating film of blade coating in the dry preceding status diagram of coating.
Fig. 3 b be blade coating graphene coating film after coating is dry status diagram.
Fig. 4 is the finished product schematic of flexibility PA graphene electromagnetic shielding material produced by the present invention.
Fig. 5 is the shielding efficiency of flexibility PA graphene electromagnetic shielding material made from embodiment three.
Appended drawing reference:
1, the PA film that sided corona treatment is crossed;2, graphene coating film.
Specific embodiment
With reference to the accompanying drawings and examples, further description of the specific embodiments of the present invention.Following embodiment is only
For clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment one:
A kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) the PA film surface of 0.02mm thickness is handled completely first, using sided corona treatment appropriate, film surface is formed carefully
Small pore-like reaches certain roughness, increases the adhesive strength of subsequent film;
(2) water-based acrylic resin, graphene slurry, defoaming agent that mass ratio is 0.9: 0.9: 0.005 are sequentially added
In vacuum mixer, adjusting negative pressure is -0.04mpa, revolving speed 1200r/min, stirs duration 12h;Graphene slurry includes stone
Black alkene, water and dispersing agent, the mass ratio of the graphene, water and dispersing agent are 25:64:1;The dispersing agent is this Lip river
The Silok-7170W type dispersing agent that Ke China provides;Defoaming agent is DQ-2209 defoaming agent, by Dongguan City a century grand plan chemical industry section
The production of skill Co., Ltd;Water-based acrylic resin commercially obtains (solid content 48%);
(3) it is calculated according to graphene stock quality, the polyether modified siloxane levelling agent for weighing 4.5% is added to step
(2) in the slurry obtained, adjusting negative pressure is -0.04mpa, revolving speed 200r/min, stirs duration 1.5h;Polyether modified siloxane
Levelling agent is GSK-550 polyether modified siloxane levelling agent, is produced by Dongguan City Gauss into Fine Chemical Co., Ltd;
(4) slurry for obtaining step (3) takes out, smooth, uniformly scratches the PA crossed in the sided corona treatment that step (1) obtains
On film, with a thickness of 0.4mm, graphene coating film 2 is formed on 1 surface of PA film that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven, drying temperature is 40 DEG C, drying time 1.5h, i.e.,
Obtain flexible PA graphene electromagnetic shielding material.
Embodiment two:
A kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) first that the processing of 0.4mm thickness PA film surface is clean, using sided corona treatment appropriate, film surface forms tiny
It is poroid, reach certain roughness, increases the adhesive strength of subsequent film;
(2) water-based acrylic resin, graphene slurry, defoaming agent that mass ratio is 1.1: 1.2: 0.008 are sequentially added
In vacuum mixer, adjusting negative pressure is -0.06mpa, revolving speed 1800r/min, and stirring duration is for 24 hours;Graphene slurry includes stone
Black alkene, water and dispersing agent, the mass ratio of the graphene, water and dispersing agent are 35:73:2;The dispersing agent is this Lip river
The Silok-7170W type dispersing agent that Ke China provides;Defoaming agent is DQ-2209 defoaming agent, by Dongguan City a century grand plan chemical industry section
The production of skill Co., Ltd;Water-based acrylic resin commercially obtains (solid content 48%);
(3) it is calculated according to graphene stock quality, the polyether modified siloxane levelling agent for weighing 5.5% is added to step
(2) in the slurry obtained, adjusting negative pressure is -0.06mpa, revolving speed 600r/min, stirs duration 3h;Polyether modified siloxane stream
Flat agent is GSK-550 polyether modified siloxane levelling agent, is produced by Dongguan City Gauss into Fine Chemical Co., Ltd;
(4) slurry for obtaining step (3) takes out, smooth, uniformly scratches the PA crossed in the sided corona treatment that step (1) obtains
On film, with a thickness of 0.8mm, graphene coating film 2 is formed on 1 surface of PA film that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven, drying temperature is 55 DEG C, drying time be 3h to get
To flexible PA graphene electromagnetic shielding material.
Embodiment three:
A kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) first that the processing of 0.2mm thickness PA film surface is clean, using front and back sides with having soaked ethanol solution when processing
Non-dust cloth wiped clean, after PA film is completely dry, then using corona machine to PA film pass through sided corona treatment appropriate, film surface shape
At uniform tiny poroid, reach certain roughness, increase the adhesive strength of subsequent film;
(2) water-based acrylic resin, graphene slurry, defoaming agent that mass ratio is 1:1:0.005 are sequentially added into vacuum
In blender (weighed when operation the water-based acrylic resin of 10g, the graphene slurry of 10g, 0.05g defoaming agent sequentially add
In vacuum mixer), adjusting negative pressure is -0.05mpa, revolving speed 1600r/min, and stirring duration is for 24 hours;In graphene slurry, institute
The mass ratio of graphene, water and dispersing agent is stated (to be provided by the production of Hunan Guo Sheng graphite Science and Technology Ltd.) for 30:69:1.Institute
Stating dispersing agent is the Silok-7170W type dispersing agent that Si Luoke China provides.Defoaming agent is DQ-2209 defoaming agent, by Dongguan City
Century-old grand plan Chemical Industry Science Co., Ltd production;Water-based acrylic resin commercially obtains (solid content 48%);
(3) it is calculated according to graphene stock quality, weighs 5% GSK-550 polyether modified siloxane levelling agent and be added to
In the slurry that step (2) obtains, adjusting negative pressure is -0.05mpa, revolving speed 400r/min, stirs duration 2h;
(4) slurry for obtaining step (3) takes out, and tests it according to quasi- GB/T1723-1993 " viscosity of the coating measuring method "
Viscosity obtains its viscosity in 20-25s;It is suitble to blade coating.Then slurry is smooth, uniformly blade coating is at the corona that step (1) obtains
On the PA film managed, with a thickness of 0.4mm, graphene coating film 2 is formed on 1 surface of PA film that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven, drying temperature is 45 DEG C, drying time be 2h to get
To flexible PA graphene electromagnetic shielding material.Its structural schematic diagram, referring to fig. 2;Finished product is as shown in Figure 4.
The water-based acrylic resin used is the main matter for scratching the film-forming after PA substrate surface, graphene conduct
Conductive materials are filled wherein, and form conductive network.Water-based acrylic resin can be shunk in solidification (referring to Fig. 3 a, figure
3b), it so as to fill graphene therein close to each other, and contacts, is more likely formed conductive channel, enhances electric conductivity, mention
High conductive stability.
The flexible PA graphene electromagnetic shielding material that step (5) is obtained carries out aging, is placed on the environment of air drying
Middle aging is for 24 hours.Later, the shielding properties of this film is tested.According to GB/T 30142-2013 (plane electromagnetic shielding material shielding
Efficiency measurement method), with coaxial flange method test material electromagnetic shielding effectiveness, in 300KHZ~1.5GHZ band limits,
Electromagnetic shielding effectiveness is 36.388~40.379dB (see Fig. 5).Specific test data is as shown in table 1:
The test of 1 electromagnet shield effect of table
The grapheme material that the present embodiment uses is a kind of highly conductive nano material, to effectively raise electromagnetic screen
Efficiency is covered, while in the case where film layer, there is good shield effectiveness, the made flexible PA graphene electromagnetism of embodiment in the same old way
Shielding material visits resistivity measurement method using four, tests to obtain resistivity≤0.1 Ω 〃 cm.
In addition, being electromagnetically shielded according to SJ/T10674-1995 (coating coating general technical specifications) to flexible PA graphene
The coating adhesion property of material, impact resistance, water resistance, resistance to temperature change, salt fog, corrosion resistance etc. are surveyed
Examination, meets the qualification standard.The results are shown in Table 2:
The detection of 2 flexibility PA graphene electromagnetic shielding material traditional performance of table
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) first that the processing of PA film surface is clean, using sided corona treatment appropriate, film surface forms tiny poroid, reaches one
Determine roughness, increases the adhesive strength of subsequent film;
It (2) is (0.9~1.1): (0.9~1.2): water-based acrylic resin, the graphene of (0.005~0.008) by mass ratio
Slurry, defoaming agent are added in vacuum mixer, and adjusting negative pressure is -0.04mpa~-0.06mpa, and revolving speed is 1200~1800r/
Min, stirring duration 12~for 24 hours;
(3) it is calculated according to graphene stock quality, the polyether modified siloxane levelling agent for weighing 4.5%~5.5% is added to step
Suddenly in the slurry that (2) obtain, adjusting negative pressure is -0.04mpa~-0.06mpa, and revolving speed is 200~600r/min, stirs duration
1.5~3h;
(4) slurry for obtaining step (3) takes out, smooth, uniformly scratches the PA film crossed in the sided corona treatment that step (1) obtains
On, with a thickness of 0.4~0.8mm, graphene coating film is formed in the PA film surface that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven to get flexibility PA graphene electromagnetic shielding material is arrived.
2. the preparation method of flexibility PA graphene electromagnetic shielding material as described in claim 1, it is characterised in that: the step
(1) in prepare PA film with a thickness of 0.02~0.4mm;Drying temperature is 40~55 DEG C in the step (5), and drying time is
1.5~3h.
3. the preparation method of flexibility PA graphene electromagnetic shielding material as claimed in claim 2, it is characterised in that: drying temperature
It is 45 DEG C, drying time 2h.
4. the preparation method of flexibility PA graphene electromagnetic shielding material as described in claim 1, it is characterised in that: the step
(2) the graphene slurry in includes graphene, water and dispersing agent, and the mass ratio of the graphene, water and dispersing agent is (25
~35): (64~73): (1~2).
5. the preparation method of flexibility PA graphene electromagnetic shielding material as claimed in claim 4, it is characterised in that: the graphite
The mass ratio of alkene, water and dispersing agent is 30:69:1.
6. the preparation method of flexibility PA graphene electromagnetic shielding material as described in claim 1, it is characterised in that: the step
(1) PA film surface is completely handled in, is the method using the non-dust cloth wiping for having soaked ethanol solution.
7. a kind of preparation method of flexibility PA graphene electromagnetic shielding material, comprising the following steps:
(1) first that the processing of 0.2mm thickness PA film surface is clean, using sided corona treatment appropriate, film surface formed it is tiny poroid,
Reach certain roughness, increases the adhesive strength of subsequent film;
(2) water-based acrylic resin, graphene slurry, defoaming agent that mass ratio is 1:1:0.005 are added in vacuum mixer,
Adjusting negative pressure is -0.05mpa, revolving speed 1600r/min, stirs duration 12h;
(3) it is calculated according to graphene stock quality, weighs 5% polyether modified siloxane levelling agent and be added to step (2) and obtain
Slurry in, adjusting negative pressure be -0.05mpa, revolving speed 400r/min, stir duration 2h;
(4) slurry for obtaining step (3) takes out, smooth, uniformly scratches the PA film crossed in the sided corona treatment that step (1) obtains
On, with a thickness of 0.4mm, graphene coating film is formed in the PA film surface that sided corona treatment is crossed;
(5) film obtained by step (4) is put and is dried into baking oven, drying temperature is 45 DEG C, and drying time is 2h soft to get arriving
Property PA graphene electromagnetic shielding material.
8. the preparation method of flexibility PA graphene electromagnetic shielding material as claimed in claim 7, it is characterised in that: the step
(2) the graphene slurry in includes graphene, water and dispersing agent, and the mass ratio of the graphene, water and dispersing agent is 30:
69:1;PA film surface is completely handled in the step (1), is using the non-dust cloth wiping for having soaked ethanol solution
Method.
9. a kind of flexibility PA graphene electromagnetic shielding material is made using such as described in any item preparation methods of claim 1-8.
10. flexible PA graphene electromagnetic shielding material described in claim 9 is in the application in electromagnetic shielding field.
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