CN111205713B - Graphene shielding film slurry and preparation method and application thereof - Google Patents
Graphene shielding film slurry and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses graphene shielding film slurry which comprises the following components in parts by weight: 3-50 parts of water-based high polymer resin; 0.1-20 parts of graphene powder; 15-35 parts of carbon black; 0.1-2 parts of carbon nano tubes; 0.1-30 parts of conductive filler; 10-30 parts of a dispersing agent; 0.5-5 parts of a functional assistant; 20-45 parts of deionized water. The slurry is prepared by simply mixing and stirring all components, takes water-based polymer resin as a carrier, and has good shielding performance after being self-dried or dried by adding graphene combined carbon nano tubes and metal materials.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding, and particularly relates to graphene shielding film slurry as well as a preparation method and application thereof.
Background
The traditional signal transmission Shielding wire (Shielding line) is formed by wrapping a signal wire by using a metal mesh-shaped braid (namely a Shielding layer), wherein the Shielding layer needs to be grounded and introduces an external interference signal into the ground, so as to achieve the purpose of Shielding, the metal mesh-shaped braid is generally red copper, tin-plated copper or braided aluminum, and the cable has the defects of thick wire diameter (including all materials such as a metal conductive core, an inner insulating skin, a filler, a PVC sheath and the like in the cable), heavy weight, high price (particularly a copper braided cable) and poor Shielding effect, so that the service performance of the cable is low, the cable cannot be suitable for the signal transmission cable with high use requirement, and particularly a 5G communication product with high signal transmission requirement.
Therefore, the inventors have endeavored to design a barrier film paste, a method of preparing the same, and applications to solve the above problems.
Disclosure of Invention
The invention aims to: the graphene shielding film slurry is prepared by taking water-based polymer resin as a carrier and adding graphene combined carbon nanotubes and a metal material, so that the graphene shielding film slurry has good shielding performance after being self-dried or dried.
Another object of the present invention is to: the preparation method of the graphene shielding film slurry is provided, the graphene shielding film slurry with good shielding performance after self-drying or drying is prepared through a simple stirring process, the cost is reduced, and the production efficiency is improved.
Yet another object of the present invention is: provided is a use of a graphene shielding film paste for a shielding layer of a signal transmission cable.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the graphene shielding film slurry comprises the following components in parts by weight:
preferably, the graphene shielding film slurry comprises the following components in parts by weight:
the aqueous high molecular resin is a main film forming material, various functional materials (powder) are bonded and fixed during film forming, and meanwhile, the high molecular resin system is aqueous, has the characteristics of environmental protection and low odor, has excellent flexibility, and can meet the flexibility requirement of cloth materials.
GraphiteAn alkene is a radical of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb-lattice two-dimensional carbon nano material, and the hexagonal honeycomb-lattice two-dimensional carbon nano material has wave absorption, shielding property and very good heat conduction performance.
The carbon black is amorphous carbon, light, loose and extremely fine black powder, has a very large surface area ranging from 10 to 3000 square meters per gram and a specific gravity of 1.8 to 2.1, has dispersibility and photostability, and can be used as a black pigment.
The carbon nano tube is used as a one-dimensional nano material, has light weight, perfect connection of a hexagonal structure, a plurality of abnormal mechanical, electrical and chemical properties, higher elastic modulus, high strength, good flexibility, fatigue resistance, isotropy and good conductivity and heat transfer performance, can be stretched, and is an ideal high-strength fiber material.
As an improvement of the graphene shielding film slurry, the aqueous high polymer resin is one of or is compounded by 100: 10-100 mass ratio of aqueous acrylic resin and aqueous PUA resin.
The aqueous acrylic resin is an acrylic resin which can be dissolved, emulsified or dispersed in water, and has excellent light, heat and chemical stability, weather resistance, chemical resistance and the like.
The waterborne PUA resin is waterborne polyurethane acrylate, wherein the molecules of the polyurethane acrylate (PUA) contain acrylic acid functional groups and urethane bonds, and the cured polyurethane has high wear resistance, adhesion, flexibility, high peel strength, excellent low-temperature resistance and excellent optical performance and weather resistance of polyacrylate, and is a resin material with excellent comprehensive performance.
As an improvement of the graphene shielding film slurry, the conductive filler is one or a mixture of at least two of nickel powder, silver powder and silver-coated copper powder in any proportion.
Preferably, the conductive filler is formed by mixing nickel powder, silver powder and silver-coated copper powder according to the mass ratio of 1-10: 0.1-1: 0.1-5.
Wherein, the nickel powder is a conductive pigment and has the function of shielding the electromagnetic interference;
the silver powder is powdery simple substance silver, has stable chemical property, low activity, high price, good heat conduction and electric conduction performance, is not easy to be corroded by chemicals, has soft quality and rich ductility, and has extremely high light reflection rate which can reach more than 99 percent.
The silver-coated copper powder is a high-conductivity filler, and the manufacturing method comprises the following steps: the chemical plating method is used to plate silver with different thickness on the surface of copper powder with certain grain diameter, namely the silver-coated copper powder, which has stable chemical property and better conductivity than the copper powder.
As an improvement of the graphene shielding film paste of the present invention, the dispersant is german digaigodisperss 750W.
German DigagteGoDispers 750W is used to increase the dispersion of the system on the powder and to stabilize it on storage.
As an improvement of the graphene shielding film slurry, the functional auxiliary agent comprises at least one of an anti-settling agent, a wetting agent, a leveling agent and an antifoaming agent;
the anti-settling agent is DISPARLON AQ-633E which is formed by locally decomposing Japanese nanmu;
the wetting agent is German basf Hydropalat WE 3220;
the leveling agent is Germany BYK-333;
the antifoaming agent is Synthron SF 561.
Preferably, the functional auxiliary agent comprises an anti-settling agent, a wetting agent, a leveling agent and a defoaming agent, and the mass ratio of the anti-settling agent to the wetting agent is 2-3: 1-2: 1.
Wherein, the native Japanese nan DISPARLON AQ-633E is used for preventing heavy particles from settling when being stored in pulp; the role of basf Hydropalat WE 3220 in germany is: during coating, the substrate is wetted; the German BYK BYK-333 has the function of improving leveling during coating; the effect of creating Synthron SF 561 in France is: when dispersed or coated, the air bubbles are eliminated.
As an improvement of the graphene shielding film slurry, the functional auxiliary agent further comprises a pH regulator, and the pH regulator is Dow Angus AMP-95 in the United states and is used for regulating the pH value of the shielding film slurry.
Preferably, the mass of the PH regulator is 5-30% of the total mass of the functional additives.
In order to achieve the other purpose, the invention adopts the technical scheme that:
a preparation method of graphene shielding film slurry comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder;
s2, placing the stirring tank on a dispersion machine for stirring, and dispersing at a high speed of 300-1200 r/min for 20-30 min to obtain the alkaline graphene shielding film slurry.
As an improvement of the preparation method of the graphene shielding film slurry, the solid content of the graphene shielding film slurry is 20% -45%, the viscosity of the graphene shielding film slurry is 60-150 gm, and the pH value of the graphene shielding film slurry is 7.5-9.5.
In order to achieve the other purpose, the invention adopts the technical scheme that:
the graphene shielding film slurry is applied to a shielding layer of a signal transmission cable, the surface resistance of the shielding layer is less than 0.20 omega/□ ASTM-D-991, and the shielding efficiency is-35 dB to-50 dB.
As an improvement of the application of the graphene shielding film slurry, the base film of the shielding layer is conductive cloth, the graphene shielding film slurry is coated on the conductive cloth through a dip-coating process, the shielding layer is formed after the graphene shielding film slurry is self-dried or dried, and the thickness of the graphene shielding film slurry after the graphene shielding film slurry is self-dried or dried is 1-3 microns.
The base material of the conductive cloth is polyester fiber, and the manufacturing method comprises the following steps: the method comprises the steps of firstly chemically depositing or physically transferring metal nickel to polyester fibers, plating a copper layer with high conductivity on the nickel, and plating nickel metal with oxidation resistance and corrosion resistance on the copper layer to form the conductive cloth, wherein the conductive cloth forms excellent conductivity and good electromagnetic shielding effect through the combination of the copper and the nickel.
The dip coating process comprises the following steps: one end of the conductive cloth penetrates through a trough of a dip-coating cylinder filled with slurry, then penetrates through a baking tunnel, is fixed on a winding roller, a machine is started, heating is started, the conductive cloth is unreeled at one end of a production line, and is coiled at the other end, the conductive cloth successively penetrates through the slurry in the dip-coating cylinder, redundant slurry is scraped by the machine, the conductive cloth penetrates through a drying area (the conductive cloth is baked for 3-5 minutes at the temperature of 60-95 ℃ or is self-dried), a shielding film is prepared by coiling, and the original thickness of a substrate is only increased by 1-3 um.
Compared with the prior art, the graphene shielding film slurry has the following technical effects: the water-based polymer resin with excellent flexibility is used as a carrier, and graphene is added to combine with the carbon nano tube and the metal material, so that the shielding film formed by self-drying or drying the shielding film slurry has good shielding performance (the application range is 100 KHz-6 GHz, the surface resistance is less than 0.20 omega/□ ASTM-D-991, the shielding effectiveness is-35 to-50 dB), thinner thickness (the wire diameter is reduced by 5-15% compared with the traditional cable) and lighter weight (the weight is reduced by 3-20% compared with the traditional cable) compared with the traditional cable.
According to the invention, the preparation method of the graphene shielding film slurry is simple, various substances mixed in the stirring cylinder are fully stirred uniformly by the dispersion machine, and the graphene shielding film slurry which is self-dried or dried and has good shielding performance, thinner thickness and lighter mass is prepared, so that the manufacturing cost is saved, the graphene shielding film slurry is suitable for batch production, and can be used as a shielding layer material of a signal transmission cable with higher shielding performance requirement.
Detailed Description
Example 1
The embodiment provides graphene shielding film slurry which comprises the following components in parts by weight:
the conductive filler is silver-coated copper powder, and the dispersant is Germany Digaogedioshper dispersions 750W; the functional additive comprises an anti-settling agent and a PH regulator, wherein the anti-settling agent is DISPARLON AQ-633E which is basically prepared from Japanese paucinations, the PH regulator is American Dow Angus ANGS AMP-95, and the weight of the PH regulator is 5% of the total weight of the functional additive.
The preparation method comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder according to the weight;
and S2, placing the stirring tank on a dispersion machine for stirring, and dispersing at a high speed of 300r/min for 30min to obtain the graphene shielding film slurry with the pH value of 7.8.
Example 2
The graphene shielding film slurry comprises the following components in parts by weight:
the conductive filler is formed by mixing nickel powder and silver-coated copper powder in a mass ratio of 2:5, the dispersant is Germany Digaogo dispers 750W, the functional auxiliary agents comprise an anti-settling agent, a wetting agent, a leveling agent and a defoaming agent in a compounding ratio of 2:1:1:1, and the anti-settling agent is a Japanese Nanmu basically synthesized into DISPARLON AQ-633E; the wetting agent is German basf Hydropalat WE 3220; the leveling agent is Germany BYK-333; the defoaming agent is French Synthron SF 561, the functional auxiliary agent further comprises a PH regulator, the PH regulator is Dow Angus ANGS AMP-95 in the United states, and the weight of the PH regulator is 10% of the total weight of the functional auxiliary agent.
The preparation method comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder according to the weight;
and S2, placing the stirring cylinder on a dispersion machine for stirring, and dispersing at a high speed of 400r/min for 27min to obtain the graphene shielding film slurry with the pH value of 8.
Example 3
The graphene shielding film slurry comprises the following components in parts by weight:
the conductive filler is prepared by compounding water-based acrylic resin and water-based PUA resin according to a mass ratio of 100:15, wherein the conductive filler is nickel powder and silver powder according to a mass ratio of 2: 0.3, the dispersant is German DigaegoDispers 750W, the functional additive comprises an anti-settling agent and a wetting agent, the compounding ratio of the anti-settling agent to the wetting agent is 3:2, the anti-settling agent is Japanese Nanhua DISPARLON AQ-633E, the wetting agent is German Pasteur Hydropalat WE 3220, the functional additive further comprises a pH regulator, the pH regulator is American Dow Angus ANGS AMP-95, and the mass of the pH regulator is 15% of the total amount of the functional additive.
The preparation method comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder;
and S2, placing the stirring tank on a dispersion machine for stirring, and dispersing at a high speed of 600r/min for 27min to obtain the graphene shielding film slurry with the pH value of 8.2.
Example 4
The graphene shielding film slurry is characterized by comprising the following components in parts by weight:
the conductive filler is formed by mixing silver powder and silver-coated copper powder in a mass ratio of 5:1, the dispersant is German Di Google dispers 750W, the functional additive comprises an anti-settling agent, a wetting agent and a leveling agent, the anti-settling agent is formed by compounding 2.5:2:1, the anti-settling agent is Japanese Nanmu basically synthesized into DISPARLON AQ-633E, the wetting agent is German Basv Hydropalat WE 3220, and the leveling agent is German BYK BYK-333; the functional auxiliary agent also comprises a PH regulator, the PH regulator is Dow Angus ANGS AMP-95 in the United states, and the mass of the PH regulator is 20% of the total mass of the functional auxiliary agent.
The preparation method comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder;
and S2, placing the stirring tank on a dispersion machine for stirring, and dispersing at a high speed of 800r/min for 25min to obtain the graphene shielding film slurry with the pH value of 8.5.
Example 5
The graphene shielding film slurry comprises the following components in parts by weight:
the conductive filler is formed by mixing nickel powder, silver powder and silver-coated copper powder in a mass ratio of 1.5:1:4, the dispersing agent is Germany DigaogoDispers 750W, the functional auxiliary agent comprises a leveling agent and an antifoaming agent in a compounding ratio of 1:1, and the leveling agent is Germany BYK BYK-333; the defoaming agent is French Synthron SF 561, the functional auxiliary agent further comprises a PH regulator, the PH regulator is Dow Angus ANGS AMP-95 in the United states, and the weight of the PH regulator is 25% of the total weight of the functional auxiliary agent.
The preparation method comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder;
and S2, placing the stirring tank on a dispersion machine for stirring, and dispersing at a high speed of 1000r/min for 23min to obtain the graphene shielding film slurry with the pH value of 9.
Example 6
1. The graphene shielding film slurry is characterized by comprising the following components in parts by weight:
the conductive filler is formed by mixing nickel powder, silver powder and silver-coated copper powder in a mass ratio of 2:1:1, the dispersing agent is Germany Digaogodi dispers 750W, the functional auxiliary agent comprises an anti-settling agent, a wetting agent and a leveling agent, and the compounding ratio of the anti-settling agent to the wetting agent to the leveling agent is 3:3: 1; the anti-settling agent is DISPARLON AQ-633E which is formed by locally decomposing Japanese nanmu; the wetting agent is German basf Hydropalat WE 3220; the leveling agent is Germany BYK BYK-333, the functional auxiliary agent further comprises a pH regulator, the pH regulator is American Dow Angus ANGS AMP-95, and the mass of the pH regulator is 30% of the total mass of the functional auxiliary agent. .
The preparation method comprises the following steps:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder;
and S2, placing the stirring cylinder on a dispersion machine for stirring, and dispersing at a high speed of 1200r/min for 20min to obtain the graphene shielding film slurry with the pH value of 9.5.
The solid content of the graphene shielding film slurry is 20% -45%, the viscosity of the graphene shielding film slurry is 60-150 gm, and the pH value of the graphene shielding film slurry is 7.5-9.5.
The graphene shielding film slurry is applied to a shielding layer of a signal transmission cable, the surface resistance of the shielding layer is less than 0.20 omega/□ ASTM-D-991, the shielding efficiency of the shielding layer is-35 to-50 dB, a base film of the shielding layer is conductive cloth, the graphene shielding film slurry is coated on the conductive cloth through a dip-coating process, the shielding layer is formed after the graphene shielding film slurry is self-dried or dried, and the thickness of the graphene shielding film slurry after the graphene shielding film slurry is self-dried or dried is 1 to 3 micrometers. Compared with the prior art, the graphene shielding film slurry is coated on the conductive cloth, and a shielding layer formed after self-drying or drying has good shielding performance (shielding effectiveness is-35 to-50 dB), thinner thickness (wire diameter is reduced by 5 to 15 percent compared with the traditional cable), lighter weight (weight is reduced by 3 to 20 percent compared with the traditional cable), and lower manufacturing cost.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention.
Claims (5)
1. The graphene shielding film slurry is characterized by comprising the following components in parts by weight:
3-50 parts of water-based high polymer resin;
0.1-20 parts of graphene powder;
15-35 parts of carbon black;
0.1-2 parts of carbon nano tubes;
0.1-30 parts of conductive filler;
10-30 parts of a dispersing agent;
0.5-5 parts of a functional assistant;
20-45 parts of deionized water;
the water-based polymer resin is one of or a mixture of water-based acrylic resin and water-based PUA resin according to a mass ratio of 100: 10-100;
the conductive filler is formed by mixing any one or at least two of nickel powder, silver powder and silver-coated copper powder in any proportion;
the dispersant is German DigaoderTEGODispers 750W;
the functional auxiliary agent comprises an anti-settling agent, a wetting agent, a flatting agent and a defoaming agent, and the mass ratio of the anti-settling agent to the wetting agent to the flatting agent is 2-3: 1-2: 1;
the anti-settling agent is DISPARLON AQ-633E which is formed by locally decomposing Japanese nanmu;
the wetting agent is German basf Hydropalat WE 3220;
the leveling agent is Germany BYK-333;
the antifoaming agent is Synthron SF 561 created in France;
the functional auxiliary agent also comprises a PH regulator, the PH regulator is Dow Angus ANGS AMP-95 in America, and the weight of the PH regulator is 5-30% of the total weight of the functional auxiliary agent.
2. The preparation method of graphene shielding film paste according to claim 1, comprising the steps of:
s1, adding the water-based polymer resin, the graphene powder, the carbon black, the carbon nano tube, the conductive filler, the dispersing agent, the functional auxiliary agent and the deionized water into a stirring cylinder;
s2, placing the stirring tank on a dispersion machine for stirring, and dispersing at a high speed of 300-1200 r/min for 20-30 min to obtain the alkaline graphene shielding film slurry.
3. The preparation method of the graphene shielding film paste according to claim 2, wherein the solid content of the graphene shielding film paste is 20% -45%, the viscosity of the graphene shielding film paste is 60-150 gm, and the pH value of the graphene shielding film paste is 7.5-9.5.
4. The application of the graphene shielding film paste according to claim 1, wherein the graphene shielding film paste is applied to a shielding layer of a signal transmission cable, the surface resistance of the shielding layer is <0.20 Ω/□ ASTM-D-991, and the shielding effectiveness is-35 dB to-50 dB.
5. The application of the graphene shielding film slurry according to claim 4, wherein a base film of the shielding layer is a conductive cloth, the graphene shielding film slurry is coated on the conductive cloth through a dip coating process, the shielding layer is formed after the graphene shielding film slurry is self-dried or dried, and the thickness of the graphene shielding film slurry after the graphene shielding film slurry is self-dried or dried is 1-3 um.
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