CN110951369A - Coating for electromagnetic shielding, preparation method and use method - Google Patents
Coating for electromagnetic shielding, preparation method and use method Download PDFInfo
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- CN110951369A CN110951369A CN201911274579.XA CN201911274579A CN110951369A CN 110951369 A CN110951369 A CN 110951369A CN 201911274579 A CN201911274579 A CN 201911274579A CN 110951369 A CN110951369 A CN 110951369A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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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
- H05K9/0092—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive pigments, e.g. paint, ink, tampon printing
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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
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- C08K2003/0806—Silver
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- 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
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- C08K2003/085—Copper
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to the technical field of electromagnetic shielding, in particular to a coating for electromagnetic shielding, a preparation method and a use method thereof. The raw materials of the coating comprise a filler and an organic carrier; wherein the organic carrier component is one or a mixture of more of polyester resin, polycarbonate, polyurethane modified epoxy resin, phenolic resin, acrylic resin and the like; the filler is one or a mixture of more of graphene, flaky silver-coated copper powder, spherical silver-coated copper powder and dendritic silver-coated copper powder; the weight percentage of the filler is 70-85 percent; the reflectivity of the coating obtained by the components is above 60 dB. According to the invention, appropriate organic carriers and fillers are preferably selected, so that the reflectivity of the coating is above 60dB, and the coating has a good shielding effect. Can be directly used, and is more flexible and convenient to use. Meanwhile, the coating obtained from the components has good corrosion resistance; low cost, environmental protection and no pollution.
Description
Technical Field
The invention relates to the technical field of electromagnetic shielding, in particular to a coating for electromagnetic shielding, a preparation method and a use method thereof.
Background
With the rapid development of the electronic information industry, communication equipment and electronic products are increasingly popularized, and the problem of electromagnetic wave interference is increasingly serious, because an electric field and a magnetic field are generated during the operation of electronic and electrical equipment, electromagnetic wave cross radiation is formed by dense arrangement and equipment devices of the electronic and electrical equipment, radiation pollution is caused, external electromagnetic interference is easily caused, the operation of the electronic and electrical equipment is seriously influenced, and an instrument or equipment of the electronic and electrical equipment generates errors, so that serious consequences are brought to the industry, families and military, and therefore, the electromagnetic shielding coating with excellent shielding performance and simple manufacturing process becomes a hotspot of research.
The electromagnetic shielding coating prevents electromagnetic energy generated by a field source from entering a shielded area by utilizing the properties of reflection, absorption and the like of the coating, can effectively eliminate or reduce the interference and influence of the electromagnetic environment on equipment and the damage to human health, and promotes various equipment to work coordinately and effectively. At present, electromagnetic shielding coatings researched and developed at home and abroad mainly adopt an additive type, a series of processes are needed to form the electromagnetic shielding coatings on a film, the electromagnetic shielding coatings cannot be directly used, the electromagnetic shielding coatings have great limitation, the thickness of products is easily increased, and the service performance of the products is influenced; the preparation process can also be relatively complex; the electromagnetic shielding effect of the coating needs to be improved.
The chinese invention patent CN104797081B discloses an electromagnetic shielding film suitable for rigid-flex boards and a manufacturing process thereof, which is a four-layer structure, comprising: the film comprises a stretched film layer, a metal film layer formed on the stretched film layer, a conductive adhesive layer coated on the metal film layer and a release protective layer attached to the conductive adhesive layer; and a slightly-adhesive protective film is attached to one surface, which is not provided with the metal film layer, of the stretched film layer to form a five-layer structure. The manufacturing process comprises the following steps: a1, removing oil stains and foreign matters on the stretched film layer, and carrying out corona treatment on the stretched film layer; a2, forming a metal film layer on the stretched film layer through vacuum sputtering, wherein the thickness is 20-3000 nm; a3, coating a conductive adhesive layer on the metal film layer, wherein the thickness is 3-15 μm, and drying in an oven at 60-120 deg.C at a linear speed of 5-30 m/min; a4, thermally adhering a delamination-type protection layer on the conductive adhesive layer; a5, rolling. Therefore, the patent discloses a specific electromagnetic shielding coating mainly of additive type, which is formed on a thin film in the manufacturing process.
Chinese patent application CN104883865A discloses a high-performance low-cost electromagnetic shielding film and a manufacturing method thereof, which includes a carrier film layer, an ink layer coated on the carrier film layer, and a conductive adhesive layer coated on the ink layer. The manufacturing method comprises the following steps: a-1, removing foreign particles on the inner surface of a carrier film roll by using a micro-adhesive wheel; a-2, coating a prepared ink layer on the inner surface of the carrier film roll; a-3, drying the ink layer by a coating oven, wherein the temperature of the coating oven is 80-180 ℃, and the linear velocity is 5-30 m/min; a-4, coating a conductive adhesive layer on the surface of the ink layer, and drying the ink layer by a coating oven, wherein the temperature of the coating oven is set to be 30-80 ℃, and the linear speed is set to be 5-30 m/min; a-5, hot-pressing and attaching a release film layer on the conductive adhesive layer; and A-6, winding into a roll. The patent discloses a specific electromagnetic shielding coating mainly of additive type, which is formed on a thin film in the manufacturing process.
The Chinese invention application CN108034313A discloses an electromagnetic shielding coating, a preparation method and an application thereof, wherein the electromagnetic shielding coating is prepared from a component A and a component B according to a molar ratio (-OH) A: (-NCO) b is 1: 1; the component A is prepared from the following raw materials in parts by weight: 25-55 parts of fluorine modified acrylic resin, 5-25 parts of elastic polyester resin, 20-30 parts of electromagnetic shielding filler, 1.5-4 parts of auxiliary agent and 5-10 parts of mixed solvent; the component B is isocyanate. The electromagnetic shielding effectiveness of the electromagnetic shielding coating prepared by the patent is less than 55 dB.
Disclosure of Invention
The invention aims to provide a coating for electromagnetic shielding, which has better shielding effect, can be directly used without film formation, and is more flexible and convenient to use.
The purpose of the invention is realized by the following technical scheme: a coating for electromagnetic shielding, the raw materials comprise filler and organic carrier;
wherein the organic carrier component is one or a mixture of more of polyester resin, polycarbonate, polyurethane modified epoxy resin, phenolic resin, acrylic resin and the like; the filler is one or a mixture of more of graphene, flaky silver-coated copper powder, spherical silver-coated copper powder and dendritic silver-coated copper powder; the weight percentage of the filler is 70-85 percent;
the reflectivity of the coating obtained by the components is above 60 dB.
The coating has good shielding effect by optimizing proper organic carriers and fillers to ensure that the reflectivity of the coating is over 60 dB. The coating can be directly used without film forming, and is more flexible and convenient to use. Meanwhile, tests show that the paint prepared from the components has good corrosion resistance.
Further, the paint reflectance is 60 to 80dB, and preferably, the paint reflectance is 61 to 75 dB.
The invention is further configured to: also comprises a curing agent, a flatting agent and a defoaming agent; wherein the curing agent comprises imidazole, boron trifluoride and DMP-30;
the mass ratio of imidazole, boron trifluoride, DMP-30, flatting agent and defoaming agent is (5-7): (2-3):3:2: 2.
By adopting the technical scheme, the curing effect is better under the synergistic action of imidazole, boron trifluoride and DMP-30, and the curing time can be better shortened. The flatting agent and the defoaming agent can control the using performance of the coating, the flatting effect is good in the using process, the treated surface is flat and smooth, and air bubbles or air holes are not easy to exist. By controlling the proportion of the curing agent, the flatting agent and the defoaming agent, the good fluidity of the coating can be kept, the curing of the coating can be accelerated, and the time is saved.
Further, the weight percentage of the curing agent is 0-5%; the weight percentage of the organic silicon flatting agent is 0-1%; the weight percentage of the defoaming agent is 0-1%;
the invention is further configured to: the organic carrier comprises polyester resin, polycarbonate, polyurethane modified epoxy resin, phenolic resin and acrylic resin, and the mass ratio of the five carriers is 20:15:50:20:5 in sequence.
Through experimental tests, the shielding effect of the technical scheme is better, and the temperature resistance of the coating can be improved.
The invention is further configured to: the filler comprises graphene, dendritic silver-coated copper powder, flaky silver-coated copper powder and spherical silver-coated copper powder; the mass ratio of the graphene to the dendritic silver-coated copper powder to the flaky silver-coated copper powder to the spherical silver-coated copper powder is 0.5:1 (0.1-0.5): 0.05.
Through test tests, the invention uses the mixed filler, the resistivity is low, and the magnetic saturation intensity is improved.
The invention is further configured to: the particle size of the graphene is less than or equal to 10 microns, the particle size of the dendritic silver-coated copper powder is less than or equal to 12 microns, the particle size of the flaky silver-coated copper powder is less than or equal to 20 microns, and the particle size of the spherical silver-coated copper powder is less than or equal to 5 microns.
By controlling the particle size of the filler, the contact area between different fillers can be increased, and the shielding effect of the coating is better.
The invention is further configured to: the viscosity of the coating is controlled to be 80-120 Pa.s, and the fineness of the coating is 5-10 mu m.
The fluidity of the coating in the using process can be better controlled by adjusting the viscosity of the coating, so that the coating is more convenient to use; by adjusting the fineness of the coating, the coating is more exquisite, and the surface of the coating is smoother after the coating is used.
The invention also aims to provide a preparation method of the coating for electromagnetic shielding, which is simple to prepare and has excellent electromagnetic shielding effect compared with the traditional coating preparation process.
The second purpose of the invention is realized by the following technical scheme: the preparation method of the coating for electromagnetic shielding in the scheme comprises the following steps:
step 1, preparing an organic carrier;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Compared with the traditional paint preparation process, the preparation method is simple to prepare, and the prepared paint has excellent electromagnetic shielding effect.
The invention is further configured to: and 2, mixing by using a three-roll grinder for 20-30min, wherein the viscosity of the prepared coating is controlled to be 80-120 Pa.s, the fineness is 8-10 mu m, and the weight percentage of solids in the coating is 70-85%.
By adopting the technical scheme, the matrix resin and the filler are uniformly mixed so as to achieve the optimal shielding effect, the viscosity of the prepared coating is controlled to be 80-120 Pa.s, and the coating is ensured to achieve good printing performance.
The third purpose of the invention is to provide a using method of the paint for electromagnetic shielding, which forms the shielding coating in a screen printing mode, and has the advantages of simple process, easy operation, environmental protection and no pollution.
The third purpose of the invention is realized by the following technical scheme: according to the application method of the paint for electromagnetic shielding, the prepared paint is printed on the PCB printed with the insulating coating in a screen printing mode, and the PCB is dried after leveling.
Compared with the traditional manufacturing process, the invention forms the shielding coating by the screen printing mode, and has simple process, easy operation, environmental protection and no pollution; the film layer formed after use has a simple structure and is formed by compounding the PCB plate, the insulating coating and the electromagnetic shielding coating, and the requirement of light weight is met.
The invention is further configured to: printing the coating on the PCB printed with the insulating coating, controlling the thickness of the slurry to be 20-30 mu m, and setting the leveling time to be 5-8 min; the constant temperature of the thermosetting is kept between 130 and 180 ℃, and the curing time is 5 to 10 min.
By adopting the technical scheme, the film layer formed after the use is simple in structure and formed by compounding the PCB, the insulating coating and the electromagnetic shielding coating, and the requirement of light weight is met. The heat curing temperature is proper, and the situation that the filler is oxidized again to influence the shielding effect due to overhigh temperature and long curing time can be avoided.
In summary, the beneficial technical effects of the present invention at least include one of the following:
1. according to the invention, appropriate organic carriers and fillers are selected, so that the fillers and the organic carriers form strong interaction, the reflectivity of the coating is above 60dB, and the coating has a good shielding effect. Can be directly used without film forming, and is more flexible and convenient to use. Meanwhile, tests show that the paint prepared from the components has good corrosion resistance; low cost, environmental protection and no pollution.
2. The invention uses the mixed filler, the resistivity is low, and the magnetic saturation intensity is improved.
3. Compared with the traditional paint preparation process, the preparation method for the electromagnetic shielding paint is simple to manufacture and convenient to use, and the prepared paint has an excellent electromagnetic shielding effect;
4. compared with the traditional paint preparation process, the preparation method for the electromagnetic shielding paint is added with polyester resin, polycarbonate, polyurethane modified epoxy resin, phenolic resin, acrylic resin and an applicable curing agent, the graphene has a large surface area, and can form a strong interface effect with a polymer due to the molecular-scale dispersion of the graphene, the graphene can be changed into a folded state due to functional groups such as hydroxyl and the like and the preparation process, and the interaction between the graphene and a polymer chain can be enhanced due to the nanoscale unevenness. The functionalized graphene surface contains chemical groups such as hydroxyl, carboxyl and the like, and can form strong hydrogen bonds with polar macromolecules such as polymethyl methacrylate, so that the graphene and silver-coated copper powder mixed filler with different morphologies are added, and the graphene composite material has the advantages of improving corrosion resistance, improving stability and shielding effect and the like.
5. The film layer formed after the coating is used has a simple structure, is formed by compounding a PCB (printed Circuit Board), an insulating coating and an electromagnetic shielding coating, and meets the requirement of light weight.
Detailed Description
Hereinafter, preferred embodiments are provided to enable those skilled in the art to better understand the present invention. However, these examples are for illustrative purposes only, and are not intended to limit the present invention to these examples.
Raw material reagent
DMP-30, the Chinese name is 2,4, 6-tris (dimethylaminomethyl) phenol; model DM, available from Nofeng Polymer materials, Inc., of Dongguan city;
urethane-modified epoxy EPU-33, cat # 19003, from advanced materials complexing (Shanghai) Inc.
Polyester resin, CAS No.: 25135-73-3, 1, 3-benzenedicarboxylic acid dimethyl ester with dimethyl-1, 4-benzenedicarboxylic acid ester and 1, 2-ethanediol;
an organosilicon leveling agent, model N-1786, from Guandong Nanhui New Material Co., Ltd;
dendritic silver-coated copper powder, model number Lis-0210, from Shenzhen Rinjin science and technology Limited;
flake silver-coated copper powder, model LI-0110, from Shenzhen Ri Hongjin science and technology Co., Ltd;
spherical silver-coated copper powder, model U-Cu-A, from Shenzhen Rinjin science and technology Limited;
the present invention is further illustrated in detail below with reference to tables and examples.
The coating for electromagnetic shielding comprises the following raw materials in parts by weight:
TABLE 1 lists of specific components and parts by weight of components for examples 1-7
Remarking: the particle size of the graphene is less than or equal to 10 microns, the particle size of the dendritic silver-coated copper powder is less than or equal to 12 microns, the particle size of the flaky silver-coated copper powder is less than or equal to 20 microns, and the particle size of the spherical silver-coated copper powder is less than or equal to 5 microns. In examples 1-4 and 6, the mass ratio of graphene, dendritic silver-coated copper powder, flaky silver-coated copper powder and spherical silver-coated copper powder was 0.5:1:0.1: 0.05; in example 5, the mass ratio of graphene, dendritic silver-coated copper powder, flaky silver-coated copper powder and spherical silver-coated copper powder was 0.5:1:0.5: 0.05;
example 1
This example 1 is intended to illustrate the preparation of a coating A for electromagnetic shielding, the fillers of the following preparation process are shown in Table 1, and the process comprises the following steps:
step 1, preparing an organic carrier; mixing an organic carrier, a curing agent, an organic silicon flatting agent and a defoaming agent GP3000, and uniformly stirring;
and 2, uniformly mixing the mixture prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 20min, wherein the viscosity of the prepared coating is controlled to be 80 Pa.s, the fineness is 5 mu m, and the weight percentage of solids in the coating is 70%.
Example 2
This example 2 is intended to illustrate the preparation of coating B for electromagnetic shielding, the fillers in the following preparation process are shown in Table 1, comprising the following steps:
step 1, preparing an organic carrier; mixing an organic carrier, a curing agent, an organic silicon flatting agent and a defoaming agent GP3000, and uniformly stirring;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 30min, wherein the viscosity of the prepared coating is controlled to be 120 Pa.s, the fineness is 10 mu m, and the weight percentage of solids in the coating is 85%.
Example 3
This example 3 is intended to illustrate the preparation of coating C for electromagnetic shielding, the fillers in the following preparation process are shown in Table 1, and the following steps are included:
step 1, preparing an organic carrier; mixing an organic carrier, a curing agent, an organic silicon flatting agent and a defoaming agent GP3000, and uniformly stirring;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 28min, wherein the viscosity of the prepared coating is controlled to be 100 pas, the fineness of the coating is 8 mu m, and the weight percentage of solids in the coating is 75%.
Example 4
This example 4 is intended to illustrate the preparation of coating D for electromagnetic shielding, the fillers in the following preparation process are shown in Table 1, and the following steps are included:
step 1, preparing an organic carrier; mixing an organic carrier, a curing agent, an organic silicon flatting agent and a defoaming agent GP3000, and uniformly stirring;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 25min, wherein the viscosity of the prepared coating is controlled to be 100 pas, the fineness of the coating is 8.5 mu m, and the weight percentage of solids in the coating is 75%.
Example 5
This example 5 is intended to illustrate the preparation of coating E for electromagnetic shielding, the fillers in the following preparation process are shown in Table 1, and the process comprises the following steps: step 1, preparing an organic carrier; mixing an organic carrier, a curing agent, an organic silicon flatting agent and a defoaming agent GP3000, and uniformly stirring;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 20min, wherein the viscosity of the prepared coating is controlled to be 110 Pa.s, the fineness is 10 mu m, and the weight percentage of solids in the coating is 75%.
Example 6
This example 1 is intended to illustrate the preparation of a coating F for electromagnetic shielding, the fillers of the following preparation being shown in Table 1, comprising the following steps:
step 1, preparing an organic carrier; mixing the organic carrier and the curing agent, and uniformly stirring;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 20min, wherein the viscosity of the prepared coating is controlled to be 120 Pa.s, the fineness is 8 mu m, and the weight percentage of solids in the coating is 75%. '
Example 7
This example 1 is intended to illustrate the preparation of a coating G for electromagnetic shielding, the fillers of the following preparation process are shown in Table 1, and the process comprises the following steps:
step 1, preparing an organic carrier; mixing an organic carrier, a curing agent, an organic silicon flatting agent and a defoaming agent GP3000, and uniformly stirring;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
Wherein the particle size of the filler graphene selected in the step 1 is 10 micrometers, the particle size of the dendritic silver-coated copper powder is 12 micrometers, the particle size of the flaky silver-coated copper powder is 20 micrometers, and the particle size of the spherical silver-coated copper powder is 5 micrometers;
and 2, mixing by using a three-roll grinder for 28min, wherein the viscosity of the prepared coating is controlled to be 100 Pa.s, the fineness is 8 mu m, and the weight percentage of solids in the coating is 73%.
The invention also carries out a comparative test, and the raw materials and the parts by weight thereof are shown in the following table 2:
TABLE 2 list of specific components and parts by weight of components for comparative examples 1-2
The obtained sample A-I was tested by a network analyzer according to GB/T25471-.
TABLE 3 tabulated reflectivity, shielding effectiveness and degree of corrosion for samples A-G
Remarking: when the reflectivity is more than or equal to 60dB and less than 65dB, the shielding effect is better; when the reflectivity is less than or equal to 65dB and less than 70dB, the shielding effect is good; when the reflectivity is less than or equal to 70dB, the shielding effect is excellent.
TABLE 4 tabulated reflectivity, shielding effectiveness and corrosion level for samples H-I
Remarking: when the reflectivity is more than or equal to 60dB and less than 65dB, the shielding effect is better; when the reflectivity is less than or equal to 65dB and less than 70dB, the shielding effect is good; when the reflectivity is less than or equal to 70dB, the shielding effect is excellent. When the reflectivity is less than 55dB, the shielding effect is not good enough and relatively poor for some special occasions.
As is clear from Table 3, the reflectance in samples A-G is above 60dB, the shielding effect is good, and further, the weight percentage of the filler is 70% -85%, so that the coating can be ensured to have good shielding effect. The sample A contains a mixture of four organic carriers, namely polyester resin, polyurethane modified epoxy resin, phenolic resin and acrylic resin, the reflectivity of the sample A is 65dB, and the shielding effect is good; in the embodiment 2, the mixture of the polycarbonate, the polyurethane modified epoxy resin, the phenolic resin and the acrylic resin is contained, the reflectivity of the sample B is 69dB, and the shielding effect is better; the shielding material of the sample C prepared by mixing the polyester resin, the polycarbonate resin, the polyurethane modified epoxy resin, the phenolic resin and the acrylic resin comprises five organic carriers, wherein the mass ratio of the five organic carriers is 20:15:50:20:5 in sequence (namely the weight ratio is 4:3:10:4:1), the shielding effect of the sample C is better, and the reflectivity reaches 72 dB. Although example 4 does not contain polycarbonate, sample D also has a good shielding effect and a reflectance of 70dB when the weight ratio of polyester resin, urethane-modified epoxy resin, phenol resin, and acrylic resin is 15:55:20: 5. In example E, the polyester resin is higher in weight portion, and the masking effect of sample E is slightly inferior to that of other samples without adding the polyurethane modified epoxy resin, but the reflectivity still reaches 61 dB. In example 6, compared to example 3, no silicone leveling agent and no defoaming agent GP3000 were added, the shielding effect of sample F was still good, the reflectance was decreased to a certain extent, but reached 66dB, and only in the use process, the leveling effect was not good enough, and bubbles were easily generated. In example 7, the ratio of each filler was greatly adjusted relative to example 3, the shielding effect was still good, and the reflectance of sample G was 67 dB.
As is clear from Table 4, in comparative example 1, although the weight ratio of the five organic carriers of polyester resin, polycarbonate, urethane-modified epoxy resin, phenol resin and acrylic resin was still 24:18:60:24:6 (i.e., the weight ratio was 4:3:10:4:1), and the mass ratio of graphene, dendritic silver-coated copper powder, flake silver-coated copper powder and spherical silver-coated copper powder was also 0.5:1:0.1:0.05, when the weight percentage of the filler in the coating was 90% or more, the printability of the resulting coating was very poor, the weight percentage of the filler was relatively decreased, the shielding effect of sample H was also very poor, and the reflectance was only 45 dB. In comparative example 2, although the weight ratio of the five organic carriers, namely the polyester resin, the polycarbonate resin, the urethane-modified epoxy resin, the phenolic resin and the acrylic resin, was still 12:9:30:13:3 (i.e., the weight ratio was 4:3:10:4:1), and the mass ratio of the graphene, the dendritic silver-coated copper powder, the flake silver-coated copper powder and the spherical silver-coated copper powder was also 0.5:1:0.1:0.05, when the weight percentage of the filler in the coating was 65% or less than 70%, the fillers could not be in sufficient contact with each other, and the conductive effect could not be achieved, thus affecting the shielding effect of sample I, and the reflectance was only 54 dB.
Example 8
The application method of the coating A for electromagnetic shielding comprises the steps of printing the prepared coating on a PCB printed with an insulating coating in a screen printing mode, leveling and drying.
The coating is printed on the PCB printed with the insulating coating, the thickness of the slurry is controlled to be 20 mu m, and the leveling time is 5 min. Thermosetting in a program control oven at 130 deg.C for 5 min.
Example 9
The application method of the coating B for electromagnetic shielding comprises the steps of printing the prepared coating on a PCB printed with an insulating coating in a screen printing mode, leveling and drying.
The coating is printed on the PCB printed with the insulating coating, the thickness of the slurry is controlled to be 30 mu m, and the leveling time is 8 min. Thermosetting in a program control oven at 180 deg.C for 10 min.
Example 10
The application method of the coating C for electromagnetic shielding comprises the steps of printing the prepared coating on a PCB printed with an insulating coating in a screen printing mode, leveling and drying.
The coating is printed on the PCB printed with the insulating coating, the thickness of the slurry is controlled to be 25 mu m, and the leveling time is 6 min. Thermosetting in a program-controlled oven at 170 deg.C for 8 min.
Example 11
The application method of the coating D for electromagnetic shielding comprises the steps of printing the prepared coating on a PCB printed with an insulating coating in a screen printing mode, leveling and drying.
The coating is printed on the PCB printed with the insulating coating, the thickness of the slurry is controlled to be 25 mu m, and the leveling time is 6 min. Thermosetting in a program-controlled oven at 170 deg.C for 8 min.
Example 12
The application method of the coating E for electromagnetic shielding comprises the steps of printing the prepared coating on a PCB printed with an insulating coating in a screen printing mode, leveling and drying.
The coating is printed on the PCB printed with the insulating coating, the thickness of the slurry is controlled to be 30 mu m, and the leveling time is 5 min. Thermosetting in a program-controlled oven at 150 deg.C for 6 min.
Example 13
The application method of the coating F for electromagnetic shielding comprises the steps of printing the prepared coating on a PCB printed with an insulating coating in a screen printing mode, leveling and drying.
The coating is printed on the PCB printed with the insulating coating, the thickness of the slurry is controlled to be 30 mu m, and the leveling time is 5 min. Thermosetting in a program-controlled oven at 150 deg.C for 6 min.
The paint panels prepared in examples 8-13 were tested according to GB/T1771-2007 in the neutral salt spray test, the results of which are shown in Table 5 below.
Table 5 corrosion performance test of paint panels prepared in examples 8-13
As is clear from Table 5, the samples prepared in examples 8 to 13 were all free from blistering and flaking of the coating film and corrosion of the substrate after the salt spray resistance test for 72 hours. The anticorrosive function of a coating can be roughly divided into two types: one is to prevent the corrosive substances outside the coating from invading into the substrate, and the other is to rely on the anticorrosion resin and the anticorrosion filler to play the role of protection and inhibition. The coating of the invention is just that the two complement each other and play the role of anticorrosion protection together. The hydroxyl, ether bond and adjacent surface in the epoxy resin generate electrostatic attraction, and the epoxy group reacts with the surface of the metal substrate to generate stable chemical bond, so that the adhesion to metal is enhanced, the formed molecular structure is compact, the medium resistance of the coating is improved, the damage of saline water, oxygen and the like to the coating is prevented, and the excellent corrosion resistance of the coating is ensured.
The salt spray corrosion resistance of H, I of comparative examples 1-2 was relatively poor, and after 72 hours of salt spray resistance, the base material of H was marked by significant corrosion and the coating film of I was foamed.
Meanwhile, tests show that the curing agent influences the temperature requirement of the coating, and the curing agent is preferably imidazole, boron trifluoride and DMP-30, so that the curing temperature of the coating on a PCB can be met, the curing time can be further shortened, and the production efficiency can be improved. The phenolic resin and the acrylic resin are added into the coating, so that the normal performance of the coating can be maintained at 260 ℃. The optimization of the particle size of the powder in the filler can increase the contact area between the powder and the powder when a plurality of fillers are mixed for use, so that the coating quality is more stable, the shielding effect is more stable, and the formed slurry is smoother when in use.
Comparative example 3
Chinese patent application CN108834391A discloses a novel composite electromagnetic shielding film for FPC and a method for manufacturing the same, wherein the shielding film manufactured in example 7 is used as comparative example 3. Compared with the invention, the preparation method is relatively complex, and the electromagnetic wave reflecting coating and the electromagnetic wave absorbing coating need to be coated on the carrier, and the shielding effect of the electromagnetic wave reflecting coating is preferably 52dB and is far lower than that of the invention.
Comparative example 4
Chinese invention patent CN105199564B discloses a thermosetting powder electromagnetic shielding coating, wherein example 1 is used as comparative example 4. Although the shielding efficiency of comparative example 4 was 90dB, which is higher than that of the present invention, the electrical resistivity was low and the magnetic saturation strength was improved by using the mixed filler of the present invention, as compared with comparative example 4. In addition, comparative example 4 prepared a powdery electromagnetic shielding coating, which was relatively complicated in preparation process and could not be directly used, and also required post-heat treatment before use. The coating is slurry, can be directly printed on a PCB printed with an insulating coating in a screen printing mode, is dried after leveling, has short curing time, greatly simplifies the preparation process, has low cost, and is environment-friendly and pollution-free.
To test the adhesion of the electromagnetic shielding coatings, the samples of examples 8-13 also passed the following tests: BS3900-E6-1992 Methods of tests for paints, Cross-cut test, ISO 2409-2013-02 Cross-cut test for paints and varnishes, ASTM D3359-09 Standard test method for adhesion by tape method, DIN 53151 test for grid cutting of coatings; the test results of the test method are that the cutting edge is completely smooth, and no square lattice falls off.
The samples of examples 10 to 11 were subjected to a load heat distortion temperature test, and after the test, no foaming, wrinkling, or peeling occurred in the coating layer on the surface of the sample.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (10)
1. The coating for electromagnetic shielding is characterized in that raw materials comprise a filler and an organic carrier;
wherein the organic carrier component is one or a mixture of more of polyester resin, polycarbonate, polyurethane modified epoxy resin, phenolic resin, acrylic resin and the like; the filler is one or a mixture of more of graphene, flaky silver-coated copper powder, spherical silver-coated copper powder and dendritic silver-coated copper powder; the weight percentage of the filler is 70-85 percent;
the reflectivity of the coating obtained by the components is above 60 dB.
2. The paint for electromagnetic shielding according to claim 1, wherein the raw materials further comprise a curing agent, a leveling agent and an antifoaming agent; wherein the curing agent comprises imidazole, boron trifluoride and DMP-30;
the mass ratio of imidazole, boron trifluoride, DMP-30, flatting agent and defoaming agent is (5-7): (2-3):3:2: 2.
3. The coating for electromagnetic shielding according to claim 1, wherein the organic vehicle comprises polyester resin, polycarbonate, urethane-modified epoxy resin, phenolic resin, and acrylic resin, and the mass ratio of the five vehicles is 20:15:50:20:5 in sequence.
4. The coating for electromagnetic shielding according to claim 1, wherein the filler comprises graphene, dendritic silver-coated copper powder, flake silver-coated copper powder, spherical silver-coated copper powder; the mass ratio of the graphene to the dendritic silver-coated copper powder to the flaky silver-coated copper powder to the spherical silver-coated copper powder is 0.5:1 (0.1-0.5): 0.05.
5. The coating for electromagnetic shielding according to claim 1, wherein the particle size of graphene is 10 μm or less, the particle size of dendritic silver-coated copper powder is 12 μm or less, the particle size of flake silver-coated copper powder is 20 μm or less, and the particle size of spherical silver-coated copper powder is 5 μm or less.
6. The paint for electromagnetic shielding according to claim 1, wherein the viscosity of the paint is controlled to 80 to 120 Pa-s, and the fineness of the paint is 5 to 10 μm.
7. The method for preparing a paint for electromagnetic shielding according to any one of claims 1 to 6, comprising the steps of:
step 1, preparing an organic carrier;
and 2, uniformly mixing the organic carrier prepared in the step 1 with a filler to obtain the electromagnetic shielding coating slurry.
8. The method of claim 7, wherein the step 2 is a three-roll mill for mixing for 20-30min, the viscosity of the prepared paint is controlled to 80-120 Pa-s, the fineness is 8-10 μm, and the weight percentage of solids in the paint is 70-85%.
9. The method of using paint for electromagnetic shielding according to any one of claims 1 to 6, wherein the prepared paint is printed on the PCB printed with the insulating coating by means of screen printing, and dried after leveling.
10. The method of claim 9, wherein the paint is printed on the PCB printed with the insulating coating, the paste thickness is controlled to be 20 μm to 30 μm, and the leveling time is 5 to 8 min; the constant temperature of the thermosetting is kept between 130 and 180 ℃, and the curing time is 5 to 10 min.
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| CN112175223A (en) * | 2020-10-14 | 2021-01-05 | 西安工程大学 | Preparation method of environment-friendly ultrathin superstructure electromagnetic shielding film |
| CN113539549A (en) * | 2021-07-15 | 2021-10-22 | 江西古川胶带有限公司 | Thermosetting conductive adhesive film and preparation method and application thereof |
| CN113604133A (en) * | 2021-08-30 | 2021-11-05 | 航天科工武汉磁电有限责任公司 | Light carbon-based electromagnetic shielding coating and preparation method thereof |
| CN114410223A (en) * | 2020-10-28 | 2022-04-29 | 中国科学院理化技术研究所 | Graphene electromagnetic shielding coating and preparation method thereof |
| CN114783654A (en) * | 2022-06-17 | 2022-07-22 | 威海云石科技有限公司 | RFID composite conductive paste, preparation method thereof and RFID electronic tag |
| CN115512874A (en) * | 2022-09-21 | 2022-12-23 | 哈尔滨工业大学（深圳） | Photovoltaic cell front silver paste and preparation method thereof, electrode and photovoltaic cell |
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| CN112175223A (en) * | 2020-10-14 | 2021-01-05 | 西安工程大学 | Preparation method of environment-friendly ultrathin superstructure electromagnetic shielding film |
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| CN113539549A (en) * | 2021-07-15 | 2021-10-22 | 江西古川胶带有限公司 | Thermosetting conductive adhesive film and preparation method and application thereof |
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| CN113604133A (en) * | 2021-08-30 | 2021-11-05 | 航天科工武汉磁电有限责任公司 | Light carbon-based electromagnetic shielding coating and preparation method thereof |
| CN114783654A (en) * | 2022-06-17 | 2022-07-22 | 威海云石科技有限公司 | RFID composite conductive paste, preparation method thereof and RFID electronic tag |
| CN115512874A (en) * | 2022-09-21 | 2022-12-23 | 哈尔滨工业大学（深圳） | Photovoltaic cell front silver paste and preparation method thereof, electrode and photovoltaic cell |
| CN116376341A (en) * | 2023-03-08 | 2023-07-04 | 安徽宇航派蒙健康科技股份有限公司 | Conductive filler, conductive film, electrothermal film and preparation method |
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