CN113388302A - Conductive coating and preparation method thereof, electronic device and manufacturing method thereof - Google Patents
Conductive coating and preparation method thereof, electronic device and manufacturing method thereof Download PDFInfo
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- 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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The embodiment of the application discloses a conductive coating and a preparation method thereof, and an electronic device and a manufacturing method thereof. The conductive coating comprises, by mass, 50-70 parts of modified hydroxy acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water. The embodiment of the application can enable a paint film/coating formed by the conductive coating to have good scratch resistance and wear resistance.
Description
Technical Field
The application relates to the field of coatings, in particular to a conductive coating and a preparation method thereof, and an electronic device and a manufacturing method thereof.
Background
At present, a great number of reports exist on the preparation of the water-based conductive coating by using graphene as a conductive filler, but in practical application, the problem of graphene agglomeration becomes the biggest limiting factor influencing the performance of the coating in conductivity.
Because the graphene has a large surface area and strong van der waals force exists between sheets, aggregation and winding phenomena are easy to occur, and the graphene cannot be stably dispersed, the graphene powder is simply used as a filler and directly added into the water-based paint, and the effect is not ideal.
Therefore, how to find a stable production method of a graphene-based water-based conductive coating, solve the problems of graphene, give full play to the performance of graphene, and enable the performance of the formed paint film to meet the high standard requirements of customers has become one of the problems to be solved by various research and development enterprises and many front-line researchers in the field.
Disclosure of Invention
The application aims to provide a conductive coating and a preparation method thereof, an electronic device and a manufacturing method thereof, which can enable a paint film/coating formed by the conductive coating to have good scratch-resistant and wear-resistant properties.
In order to solve the above problems, the technical solution of the embodiment of the present application is as follows:
the conductive coating comprises, by mass, 50-70 parts of modified hydroxyl acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resistant agent and 0-40 parts of water.
A method for preparing an electrically conductive coating, the method comprising: step S1, providing 50-70 parts of modified hydroxyl acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water by mass; step S2, mixing 50-70 parts of modified hydroxyl acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water to obtain the conductive coating.
In the above method for preparing a conductive paint, the step S2 includes: firstly, mixing the modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and water, and then sequentially adding the graphene slurry, a defoaming agent, a wetting agent, a leveling agent and an anti-wear agent for mixing treatment to obtain the conductive coating.
In the above method for preparing a conductive paint, the step S2 includes: step S21, adding the modified hydroxyl acrylic acid secondary dispersion, amino resin, dispersant and deionized water into a dispersion cylinder according to the formula and the set amount; step S22, uniformly stirring the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent and the deionized water in the dispersion cylinder; step S23, adding graphene slurry into the dispersion cylinder; step S24, uniformly dispersing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water and the graphene slurry in the dispersion cylinder; step S25, when dispersing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water and the graphene slurry in the dispersion cylinder, respectively adding a defoaming agent, a wetting agent, a leveling agent, an anti-wear agent and the balance of deionized water into the dispersion cylinder; and step S26, dispersing the modified hydroxy acrylic acid secondary dispersion, amino resin, dispersing agent, deionized water, graphene slurry, defoaming agent, wetting agent, leveling agent and wear-resisting agent in the dispersion cylinder uniformly at a high speed.
In the above method for preparing a conductive paint, after the step S26, the step S2 further includes: and step S27, filtering the mixture of the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water, the graphene slurry, the defoaming agent, the wetting agent, the leveling agent and the wear-resisting agent in the dispersion cylinder to obtain the conductive coating.
In the above method for preparing a conductive paint, before the step S1, the method further includes: step S3, preparing modified hydroxy acrylic acid secondary dispersion.
In the above method for preparing a conductive paint, the step S3 includes: step S31, placing a predetermined weight of hydroxyl acrylic acid secondary dispersion into a reaction kettle; step S32, adding anhydrous ethyl acetate with the same weight as the secondary hydroxyl acrylic acid dispersoid into the reaction kettle, and uniformly stirring; step S33, according to (-COOH): (-OH) ═ 1:3 trimethoxysilanecarboxylic acid was added; step S34, heating to 85 ℃ under the protection of nitrogen; step S35, adding dibutyltin dilaurate accounting for 0.5% of the total weight of the mixture of the hydroxyacrylic acid secondary dispersion, the anhydrous ethyl acetate and the trimethoxy silane formic acid into the reaction kettle to accelerate catalytic reaction, wherein the reaction time is 2.5 hours to 3.5 hours.
An electronic device comprising an electronic device body and the above conductive coating layer, the conductive coating layer being provided on a surface of the electronic device body.
A method of manufacturing an electronic device, the method comprising: step S4, coating the conductive paint on the surface of the electronic device main body; step S5, performing a drying process on the conductive paint applied on the surface of the electronic device main body to form a conductive coating on the surface of the electronic device main body.
In the above method of manufacturing an electronic device, the temperature at which the conductive coating material coated on the surface of the electronic device main body is dried is 160 ℃ to 180 ℃, and the drying time is 30 minutes to 40 minutes.
According to the embodiment of the invention, the modified hydroxy acrylic acid secondary dispersion and the amino resin are combined according to a specific proportion to be used as the matrix resin of the conductive coating, wherein the modified hydroxy acrylic acid secondary dispersion is used as a main film forming substance and a crosslinking carrier, the amino resin is used as a crosslinking curing agent and is crosslinked and cured with the modified hydroxy acrylic acid secondary dispersion, so that the crosslinking density of a paint film/coating formed by the conductive coating can be improved, and the hardness and scratch resistance of the paint film/coating can be further improved by adding the wear-resisting agent, so that the paint film/coating formed by the conductive coating has good scratch resistance and wear resistance.
Drawings
Fig. 1 is a flow chart of a method for preparing a conductive coating according to an embodiment of the present invention.
Fig. 2 is a flowchart of the step of mixing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the graphene slurry, the defoaming agent, the wetting agent, the leveling agent, the wear-resistant agent and the water in fig. 1 to obtain the conductive coating.
FIG. 3 is a flow chart of the steps for preparing the modified hydroxy acrylic acid secondary dispersion in the method for preparing the conductive coating provided by the embodiment of the present invention.
Fig. 4 is a flowchart of a method for manufacturing an electronic device according to an embodiment of the present invention.
Detailed Description
In order to make the purpose, technical solution and technical effect of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below. The embodiments described below are some, but not all embodiments of the invention. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention. Those whose specific conditions are not specified in the examples are carried out according to conventional conditions or conditions recommended by the manufacturer; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be understood that the weight of the related components mentioned in the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, it is within the scope of the disclosure that the content of the related components is scaled up or down according to the embodiments of the present invention. Specifically, the weight described in the embodiments of the present invention may be a unit of mass known in the chemical field such as μ g, mg, g, kg, etc.
In addition, unless the context clearly uses otherwise, an expression of a word in the singular is to be understood as including the plural of the word. The terms "comprises" or "comprising" are intended to specify the presence of stated features, quantities, steps, operations, elements, portions, or combinations thereof, but are not intended to preclude the presence or addition of one or more other features, quantities, steps, operations, elements, portions, or combinations thereof.
The embodiment of the invention provides a conductive coating which comprises, by mass, 50-70 parts of modified hydroxyl acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water.
The conductive coating provided by the embodiment of the invention comprises a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent, graphene, a defoaming agent, a wetting agent, a leveling agent, an anti-wear agent and water, wherein the graphene is a conductive component, the modified hydroxyl acrylic acid secondary dispersion, the amino resin, the graphene and the anti-wear agent are jointly combined to serve as an anti-wear component (the modified hydroxyl acrylic acid secondary dispersion and the amino resin serve as main film forming components), the anti-wear agent is a main enhanced paint film/coating anti-scraping and anti-wear component, and other auxiliary agents and water are matched, so that a coating formed by the conductive coating provided by the embodiment of the invention has good anti-scraping, anti-wear performance and conductivity; secondly, all components in the conductive coating provided by the embodiment of the invention are environment-friendly components, so that the conductive coating is a water-based environment-friendly coating and has the advantage of environmental friendliness; finally, although the conductive coating provided by the embodiment of the invention is a water-based coating, the hardness of the conductive coating formed by the conductive coating is greater than or equal to 4H, is equivalent to that of an oil-based coating, is more weather-resistant than the traditional conductive coating, and can be applied to various scenes such as indoor and outdoor scenes.
Specifically, the modified hydroxyl acrylic acid secondary dispersion is hydroxyl acrylic ester secondary dispersion which takes water as a dispersion medium and has a self-emulsifying function, can be mixed with aliphatic polyisocyanate to prepare varnish and finish paint, and can also be mixed with amino resin or blocked polyisocyanate to prepare the water-based single-component industrial baking coating.
Preferably, the hydroxyl acrylic acid secondary dispersion is DB3642 produced by Hubei double bond fine chemical engineering company, which has excellent fullness, glossiness and chemical resistance and good toughness and hardness combination property and is commonly used for water-based baking paint. The process for modifying DB3642 is as follows: trimethoxy silane formic acid is used as a modifying functional agent, and carboxyl (-COOH) of an organic silicon compound and hydroxyl (-OH) of the DB3642 hydroxyacrylic acid secondary dispersion are subjected to esterification reaction to produce (-COO-) groups, so that the trimethoxy silane formic acid is grafted into the DB3642 hydroxyacrylic acid secondary dispersion to effectively improve the weather resistance, solvent resistance, adhesive force and high and low temperature flexibility of the modified resin; the reaction principle is as follows:
specifically, the preparation method of the modified hydroxy acrylic acid secondary dispersion (method for modifying DB3642 hydroxy acrylic acid secondary dispersion) comprises the following steps: putting a predetermined weight of the second-stage hydroxy acrylic acid dispersion into a reaction kettle, adding anhydrous ethyl acetate with equal weight, uniformly stirring, and then according to the formula (-COOH): adding trimethoxy silane formic acid into (-OH) ═ 1:3, starting condensation reflux, heating to 85 ℃ under the protection of nitrogen, and in order to shorten the reaction time, dropwise adding dibutyltin dilaurate accounting for 0.5 percent of the total weight of the materials to accelerate the catalytic reaction, and obtaining the modified DB3642 hydroxyacrylic acid secondary dispersion after the reaction is carried out for about 3 hours.
The amino resin is a resin having a plurality of functional groups, which is obtained by polycondensing an amino group-containing compound with aldehydes and alcohols. The amino resin is Resimene747 produced by INEOS, is a commercial-grade hexamethoxy methyl melamine resin, is in a liquid state, has the non-volatile content of more than 98 percent, is used as a cross-linking agent of various polymer materials, and has excellent performance.
The abrasion resistance agent is a water-dispersible, ultra-high molecular weight polydimethylsiloxane dispersion for increasing the smoothness and abrasion resistance of the conductive coating. The wear-resistant agent is a smooth scratch-resistant auxiliary agent MD-2000 produced by Westol Kerr, belongs to high-density polyethylene wax, can reduce friction coefficient, prevent adhesion and improve wear resistance and nail scratch resistance, has good compatibility with acrylic resin, can be directly added into an acrylic resin system, and has a synergistic effect with DB3642 (DB3642 is used as a carrier of a main film forming substance and provides basic paint film performance, the MD-2000 is further optimized on the aspect of paint film surface performance and provides a more smooth texture paint film, and the two play main roles in paint film hardness, wear resistance and scratch resistance), so that the obtained conductive paint has superior hardness, wear resistance and scratch resistance. The wear-resistant agent mainly plays a role in improving the smoothness of a paint film of the conductive paint, can reduce the friction coefficient of the paint film, prevent adhesion and improve the wear-resistant and nail-scraping-resistant performances, and the addition amount is 0.3-5 parts (the wear-resistant performance is not obviously improved when the addition amount is small).
The graphene is SE4101 produced by Hexagon materials GmbH, and the addition amount of the graphene in the conductive coating determines the conductive effect of the conductive coating. The graphene generally has certain thixotropy, so that when the addition amount is too high, the viscosity of the obtained conductive coating is easily greatly increased, and the constructability and the leveling property of the conductive coating are seriously influenced; the addition amount of the graphene is too low, and the expected conductive effect cannot be achieved. Therefore, in the embodiment of the invention, the content of the graphene in the conductive coating is controlled to be 10-30 parts, so that the conductive coating has good conductivity and constructability.
The auxiliary agent is used as an auxiliary material in the conductive coating, and has the effects of improving the performance of the conductive coating, promoting the film formation of a coating and the like. The auxiliary agent comprises a defoaming agent and/or a dispersing agent.
Wherein the defoaming agent can reduce bubbles formed by entrainment of air in the conductive coating material or suppress bubble generation. The defoaming agent is TEGO 902W (polyether polysiloxane emulsion) produced by Germany Digao auxiliary agent company, and has the advantages of good defoaming effect and no influence on leveling. The defoaming agent is 0.05 to 0.2 parts by weight (the defoaming effect is poor when the addition amount is small, and the paint film has the defects of poor paint film such as miliaria, foaming, shrinkage cavity and the like due to more foaming in the construction process/paint film drying process, and the bad phenomena such as oil pits, shrinkage cavity and the like are easy to occur when the addition amount is too large).
The dispersing agent is helpful for improving the dispersibility of each component in the conductive coating, and avoids the occurrence of layering and mutual aggregation among particles. The BYK-190 aqueous polymer dispersant which is matched with SE4101 graphene and produced by Bick company is selected as the dispersant, the dispersant can prevent the components of the conductive coating from flocculating, the stability and the tinting strength of the obtained conductive coating are improved, the storage stability of the conductive coating is improved, the wettability and the glossiness of the conductive coating are improved, and the viscosity of the conductive coating is reduced.
The wetting agent can spread the conductive coating on the surface of a coated material or penetrate the surface of the coated material by reducing the surface tension or the interfacial tension of the conductive coating, so that the coated material is wetted to achieve a good coating effect, and the addition amount of the wetting agent is 0.05-0.1 part (if the addition amount is small, the wettability and the permeability of the conductive coating are insufficient, so that the paint film adhesion is insufficient).
BYK333 is selected as the leveling agent, BYK333 is an organosilicon surfactant which has the functions of strongly reducing surface tension and obviously improving the wetting capacity of a base material, can prevent surface defects such as shrinkage, pinholes, bubbles and orange peel, can prevent implosion and improve leveling, and the addition amount of the leveling agent is 0.1-0.3 part by mass (the addition amount is too small, so that the smoothness of a paint film is poor, and the addition amount is too large, so that the defoaming property and the interlayer/recoating adhesion are poor).
The water is used as a solvent of the conductive coating provided by the embodiment of the invention, so that the conductive coating is an environment-friendly water-based coating, does not contain harmful substances such as benzene and toluene, and is more environment-friendly. As an improvement, the water is deionized water, that is, deionized water is selected as a solvent, which is beneficial to reducing the surface tension of the obtained conductive coating.
According to the embodiment of the invention, the modified hydroxy acrylic acid secondary dispersion and the amino resin are combined according to a specific proportion to be used as the matrix resin of the conductive coating, wherein the modified hydroxy acrylic acid secondary dispersion is used as a main film forming substance and a crosslinking carrier, the amino resin is used as a crosslinking curing agent and is crosslinked and cured with the modified hydroxy acrylic acid secondary dispersion, so that the crosslinking density of a paint film/coating formed by the conductive coating can be improved, and the hardness and scratch resistance of the paint film/coating can be further improved by adding the wear-resisting agent, so that the paint film/coating formed by the conductive coating has good scratch resistance and wear resistance.
Compared with the adoption of other metal conductive fillers, the embodiment of the invention adopts the graphene as the conductive filler, so that the prepared water-based conductive coating has more excellent conductive performance, and simultaneously, the graphene has the advantages of larger specific surface area, high strength and the like, so that the corrosion resistance, the mechanical property and the like of the conductive coating product can be optimized. Due to the characteristics of high conductivity, strong mechanical property and the like, the prepared conductive coating has the characteristics of good conductivity, low cost, non-toxic or low-toxicity raw materials, high bonding fastness with a base material and convenience in use, so that the conductive coating can gradually replace part of metal to be used as a conductive material and can be applied to the fields of intelligent textiles, photovoltaic industry, printed circuits, biosensors, electromagnetic shielding materials, conductivity, RFID antennas, aviation and the like.
Correspondingly, the embodiment of the invention provides a preparation method of a conductive coating, which comprises the following steps:
and step S1, providing a modified hydroxyl acrylic acid secondary dispersion, amino resin, an anti-wear agent, graphene slurry, an auxiliary agent and water. Specifically, 50-70 parts of modified hydroxy acrylic acid secondary dispersion, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water are provided according to parts by mass.
And step S2, mixing the modified hydroxyl acrylic acid secondary dispersion, amino resin, a wear-resisting agent, graphene slurry, an auxiliary agent and water to obtain the conductive coating. Specifically, 50-70 parts of modified hydroxy acrylic acid secondary dispersion, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water are mixed to obtain the conductive coating.
In the preparation method of the conductive coating provided by the embodiment of the invention, the conductive coating with the functions can be obtained by mixing the raw materials according to a specific ratio, and the preparation method has the advantages of simplicity, easiness and convenience in implementation.
The surface tension of the obtained conductive coating is more uniform and the components are uniformly dispersed by adding and mixing the components according to a specific sequence, so that the problem of oil leakage of a coating formed by the conductive coating is solved (the components are not uniformly dispersed, particularly, when a surfactant influencing the surface tension of a paint film is not sufficiently and uniformly dispersed, the oil leakage phenomenon is easy to occur, and the dispersion sequence is very important).
The step S2 includes: firstly, mixing the modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and water, and then sequentially adding the graphene slurry, a defoaming agent, a wetting agent, a leveling agent and an anti-wear agent for mixing treatment to obtain the conductive coating.
Specifically, step S2 includes:
and step S21, adding the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent and the deionized water into the dispersing cylinder according to the formula and the set amount.
And step S22, uniformly stirring the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent and the deionized water in the dispersion cylinder.
And step S23, adding graphene slurry into the dispersion cylinder.
And step S24, uniformly dispersing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water and the graphene slurry in the dispersion cylinder.
And step S25, respectively adding a defoaming agent, a wetting agent, a leveling agent, an anti-wear agent and the balance of deionized water into the dispersing cylinder when dispersing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water and the graphene slurry in the dispersing cylinder.
And step S26, dispersing the modified hydroxy acrylic acid secondary dispersion, amino resin, dispersing agent, deionized water, graphene slurry, defoaming agent, wetting agent, leveling agent and wear-resisting agent in the dispersion cylinder uniformly at a high speed.
Firstly adding a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and deionized water as a dispersing carrier, adding graphene slurry for the second time for better uniform arrangement of graphene, and then adding a defoaming agent, a wetting agent and a leveling agent under the condition of high-speed dispersion for avoiding the phenomenon of paint film shrinkage caused by non-uniform dispersing aids, wherein the rest is added finally.
After the step S26, the step S2 further includes:
and step S27, filtering the mixture of the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water, the graphene slurry, the defoaming agent, the wetting agent, the leveling agent and the wear-resisting agent in the dispersion cylinder to obtain the conductive coating.
Prior to the step S1, the method further includes:
step S3, preparing modified hydroxy acrylic acid secondary dispersion.
The step S3 includes:
step S31, placing a predetermined weight of hydroxyl acrylic acid secondary dispersion into a reaction kettle;
step S32, adding anhydrous ethyl acetate with the same weight as the secondary hydroxyl acrylic acid dispersoid into the reaction kettle, and uniformly stirring;
step S33, according to (-COOH): (-OH) ═ 1:3 trimethoxysilanecarboxylic acid was added;
step S34, heating to 85 ℃ under the protection of nitrogen;
step S35, adding 0.5% of dibutyltin dilaurate based on the total weight of the mixture of the secondary hydroxyl acrylic dispersion, the anhydrous ethyl acetate and the trimethoxy silane formic acid to the reaction kettle to accelerate the catalytic reaction for a reaction time of 2.5 hours to 3.5 hours (e.g., 3 hours).
Example 1
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
10 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
24.5 parts of water.
(2) Mixing materials: firstly, adding a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and 20% deionized water into a dispersion cylinder, wherein the amount of the modified hydroxyl acrylic acid secondary dispersion is set according to a formula, fully stirring uniformly, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water according to the set amount of the formula in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Example 2
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
60 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
10 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
14.5 parts of water.
(2) Mixing materials: firstly, adding a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and 20% deionized water into a dispersion cylinder, wherein the amount of the modified hydroxyl acrylic acid secondary dispersion is set according to a formula, fully stirring uniformly, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water according to the set amount of the formula in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Example 3
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
70 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
10 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
4.5 parts of water.
(2) Mixing materials: firstly, adding a formula-set amount of modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and deionized water into a dispersion cylinder, fully and uniformly stirring, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding the formula-set amount of a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Example 4
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
60 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
20 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
4.5 parts of water.
(2) Mixing materials: firstly, adding a formula-set amount of modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and deionized water into a dispersion cylinder, fully and uniformly stirring, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding the formula-set amount of a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Example 5
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
30 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
4.5 parts of water.
(2) Mixing materials: firstly, adding a formula-set amount of modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and deionized water into a dispersion cylinder, fully and uniformly stirring, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding the formula-set amount of a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Example 6
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
30 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
4.8 parts of an anti-wear agent;
2 parts of water.
(2) Mixing materials: firstly, adding a formula-set amount of modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and deionized water into a dispersion cylinder, fully and uniformly stirring, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding the formula-set amount of a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Comparative example 1
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
30 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
0 part of an anti-wear agent;
6.8 parts of water.
(2) Mixing materials: firstly, adding a formula-set amount of modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and deionized water into a dispersion cylinder, fully and uniformly stirring, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding the formula-set amount of a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Comparative example 2
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
20 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
14.5 parts of water.
(2) Mixing materials: firstly, adding a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and 10% deionized water into a dispersion cylinder, wherein the amount of the modified hydroxyl acrylic acid secondary dispersion is set according to a formula, fully stirring uniformly, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water according to the set amount of the formula in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Comparative example 3
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
10 parts of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
24.5 parts of water.
(2) Mixing materials: firstly, adding a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and 10% deionized water into a dispersion cylinder, wherein the amount of the modified hydroxyl acrylic acid secondary dispersion is set according to a formula, fully stirring uniformly, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water according to the set amount of the formula in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Comparative example 4
The preparation method of the conductive coating comprises the following steps:
(1) preparing materials: preparing modified hydroxyl acrylic acid secondary dispersoid, a wear-resisting agent, amino resin, graphene slurry, an auxiliary agent (a dispersing agent, a defoaming agent, a wetting agent and a flatting agent) and deionized water according to the following parts by mass:
50 parts of a modified hydroxyacrylic acid secondary dispersion;
10 parts of an amino resin;
3 parts of a dispersant;
0 part of graphene slurry;
0.05 part of a defoaming agent;
0.05 part of wetting agent;
0.1 part of a leveling agent;
2.3 parts of an anti-wear agent;
34.5 parts of water.
(2) Mixing materials: firstly, adding a modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and 10% deionized water into a dispersion cylinder, wherein the amount of the modified hydroxyl acrylic acid secondary dispersion is set according to a formula, fully stirring uniformly, then adding graphene slurry, dispersing for 30 minutes at a high speed, respectively adding a defoaming agent, a wetting agent, a flatting agent, an abrasion-resistant agent and the balance of deionized water according to the set amount of the formula in sequence under the condition of high-speed dispersion, dispersing for 30 minutes at a high speed again, and filtering by using a 300-mesh filter screen to obtain the conductive coating.
Performance testing and results
1. The conductive coatings obtained in examples 1-6 and comparative examples 1-4 were coated with an aluminum-based conductive sheet (conductive sheet for chip) respectively (dry film thickness about 20 μm, too thin paint film is insufficient to sufficiently exhibit paint film properties such as reduced rubbing times and easy to show bottom, and paint film thickness is too thick and easy to cause sagging and increase unnecessary construction costs), baked at 160 ℃ for 30 minutes until completely dried to form a coating, and the surface thereof was rubbed with 99.5% absolute ethyl alcohol at 500g pressure back and forth for 1000 times, wherein the coatings of examples 1-6 and comparative examples 2-4 have no bottom, and the coating of comparative example 1 has bottom (poor alcohol resistance rubbing ability).
2. Taking an aluminum-based conductive sheet (conductive sheet of a chip), respectively coating the conductive coatings obtained in examples 1-6 and comparative examples 1-4, baking at 160 ℃ for 30 minutes until completely drying to form a coating, and carrying out an abrasion resistance test on the coating with an RCA-resistant paper tape at 300g force for 200 times, wherein the coatings of examples 1-6 and comparative examples 2-4 have no open bottom, and the coating of comparative example 1 has open bottom (a paint film is damaged and exposed when the conventional conductive coating is rubbed for 50 times), wherein the abrasion resistance test of example 6 can exceed 600 times, and the abrasion resistance performance is obviously better than that of the rest examples and comparative examples.
3. The conductive coatings obtained in examples 1 to 6 and comparative examples 1 to 4 were coated on aluminum-based conductive sheets (conductive sheets for chips), respectively, and baked at 160 ℃ for 30 minutes until completely dried to form coatings, and subjected to a Baige adhesion test. As a result: adhesion rating 0 (ISO standard); the coating hardness of examples 1 to 6 and comparative examples 1 to 4 was 4H or more. The coating obtained in example 6 had the most smooth hand, and the coating obtained in comparative example 1 had a drier hand.
4. Taking an aluminum-based conductive sheet (conductive sheet of a chip), respectively coating the conductive coatings obtained in examples 1 to 6 and comparative examples 1 to 4, baking the conductive coatings at 160 ℃ for 30 minutes until the conductive coatings are completely dried to form coatings, and measuring the surface resistance data as follows:
embodiments of the present invention also provide an electronic device including an electronic device body and a conductive coating disposed on a surface of the electronic device body.
The conductive coating is formed by coating the conductive coating on the surface of an electronic device main body and drying the conductive coating, wherein the temperature for drying the conductive material is set to be 160 ℃ to 180 ℃ in combination with the temperature required for curing the resin in the conductive coating, and the typical but non-limiting drying temperature is 160 ℃, 161 ℃, 162 ℃, 163 ℃, 164 ℃, 165 ℃, 166 ℃, 167 ℃, 168 ℃, 169 ℃, 170 ℃, 171 ℃, 172 ℃, 173 ℃, 174 ℃, 175 ℃, 176 ℃, 177 ℃, 178 ℃, 179 ℃ and 180 ℃, so that the formation of the coating can be accelerated, and the hardness of the coating and the bonding strength between the coating and a conductive device can be improved; in addition, the time for drying the conductive material is set to be 30 minutes to 40 minutes, and typical but not limiting drying time is 30 minutes, 31 minutes, 32 minutes, 33 minutes, 34 minutes, 35 minutes, 36 minutes, 37 minutes, 38 minutes, 39 minutes, 40 minutes, so that the graphene coating has sufficient hardness and the bonding strength between the graphene coating and the conductive device is improved.
The conductive coating is used to enable charge transfer between the electronic device body and an external object in contact with the conductive coating.
The electronic device body according to the embodiment of the present invention includes, but is not limited to, a conductive silicone connector (zebra strip), a hot-press conductive zebra paper, a conductive rubber strip, a conductive rubber plate, a conductive silicone key, and a rubber precision component. The conductive coating is widely applied to weak current electronic products such as mobile phones, game machines, telephones, electronic watches, calculators, instruments, remote controllers, thermometers, computer keyboards, medical care, liquid crystal displays and the like. The electronic device main body can be a conducting strip, a conducting tube and the like; the substrate of the electronic device main body may be a variety of suitable materials, wherein, when the substrate is a metal, particularly aluminum or an alloy material containing aluminum, the bonding force with the conductive coating material is better.
The embodiment of the invention also provides a manufacturing method of the electronic device, which comprises the following steps:
step S4, coating the conductive paint on the surface of the electronic device main body;
and step S5 of drying the conductive paint coated on the surface of the electronic device main body to form a conductive coating on the surface of the electronic device main body, wherein the temperature of drying the conductive paint coated on the surface of the electronic device main body is 160 to 180 ℃, and the drying time is 30 to 40 minutes.
The conductive coating provided by the embodiment of the invention has good scratch resistance, wear resistance, conductivity and weather resistance, and when used as a conductive coating of an electronic device, the conductive coating can provide a good conductive effect for the electronic device, can avoid the problems of paint dropping and the like caused by overlong service time of the electronic device, and is suitable for various scenes such as indoor and outdoor scenes, so that the conductive coating has good application prospect and market value.
In summary, although the present application has been described with reference to the preferred embodiments, the above-described preferred embodiments are not intended to limit the present application, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present application, so that the scope of the present application shall be determined by the appended claims.
Claims (10)
1. The conductive coating is characterized by comprising, by mass, 50-70 parts of modified hydroxyl acrylic acid secondary dispersion, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of leveling agent, 0.3-5 parts of wear-resistant agent and 0-40 parts of water.
2. A preparation method of a conductive coating is characterized by comprising the following steps:
step S1, providing 50-70 parts of modified hydroxyl acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water by mass;
step S2, mixing 50-70 parts of modified hydroxyl acrylic acid secondary dispersoid, 10-20 parts of amino resin, 3-8 parts of dispersing agent, 10-50 parts of graphene slurry, 0.05-0.2 part of defoaming agent, 0.05-0.1 part of wetting agent, 0.1-0.3 part of flatting agent, 0.3-5 parts of wear-resisting agent and 0-40 parts of water to obtain the conductive coating.
3. The method for preparing the conductive paint according to claim 2, wherein the step S2 includes: firstly, mixing the modified hydroxyl acrylic acid secondary dispersion, amino resin, a dispersing agent and water, and then sequentially adding the graphene slurry, a defoaming agent, a wetting agent, a leveling agent and an anti-wear agent for mixing treatment to obtain the conductive coating.
4. The method for preparing the conductive paint according to claim 2 or 3, wherein the step S2 includes:
step S21, adding the modified hydroxyl acrylic acid secondary dispersion, amino resin, dispersant and deionized water into a dispersion cylinder according to the formula and the set amount;
step S22, uniformly stirring the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent and the deionized water in the dispersion cylinder;
step S23, adding graphene slurry into the dispersion cylinder;
step S24, uniformly dispersing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water and the graphene slurry in the dispersion cylinder;
step S25, when dispersing the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water and the graphene slurry in the dispersion cylinder, respectively adding a defoaming agent, a wetting agent, a leveling agent, an anti-wear agent and the balance of deionized water into the dispersion cylinder;
and step S26, dispersing the modified hydroxy acrylic acid secondary dispersion, amino resin, dispersing agent, deionized water, graphene slurry, defoaming agent, wetting agent, leveling agent and wear-resisting agent in the dispersion cylinder uniformly at a high speed.
5. The method of preparing the conductive paint as claimed in claim 4, wherein the step S2 further includes, after the step S26:
and step S27, filtering the mixture of the modified hydroxy acrylic acid secondary dispersion, the amino resin, the dispersing agent, the deionized water, the graphene slurry, the defoaming agent, the wetting agent, the leveling agent and the wear-resisting agent in the dispersion cylinder to obtain the conductive coating.
6. The method for preparing the conductive paint according to claim 2, wherein before the step S1, the method further comprises:
step S3, preparing modified hydroxy acrylic acid secondary dispersion.
7. The method for preparing the conductive paint according to claim 6, wherein the step S3 includes:
step S31, placing a predetermined weight of hydroxyl acrylic acid secondary dispersion into a reaction kettle;
step S32, adding anhydrous ethyl acetate with the same weight as the secondary hydroxyl acrylic acid dispersoid into the reaction kettle, and uniformly stirring;
step S33, according to (-COOH): (-OH) ═ 1:3 trimethoxysilanecarboxylic acid was added;
step S34, heating to 85 ℃ under the protection of nitrogen;
step S35, adding dibutyltin dilaurate accounting for 0.5% of the total weight of the mixture of the hydroxyacrylic acid secondary dispersion, the anhydrous ethyl acetate and the trimethoxy silane formic acid into the reaction kettle to accelerate catalytic reaction, wherein the reaction time is 2.5 hours to 3.5 hours.
8. An electronic device comprising an electronic device body and the conductive coating of claim 1 disposed on a surface of the electronic device body.
9. A method of manufacturing an electronic device, comprising:
step S4, coating the conductive paint on the surface of the electronic device main body;
step S5, performing a drying process on the conductive paint applied on the surface of the electronic device main body to form a conductive coating on the surface of the electronic device main body.
10. The method of manufacturing an electronic device according to claim 9, wherein the temperature at which the conductive paint applied to the surface of the electronic device main body is dried is 160 ℃ to 180 ℃ and the drying time is 30 minutes to 40 minutes.
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