CN116376372A - Super-hydrophobic treatment composite material for surface of printed circuit board and preparation and use methods thereof - Google Patents
Super-hydrophobic treatment composite material for surface of printed circuit board and preparation and use methods thereof Download PDFInfo
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- CN116376372A CN116376372A CN202310568799.3A CN202310568799A CN116376372A CN 116376372 A CN116376372 A CN 116376372A CN 202310568799 A CN202310568799 A CN 202310568799A CN 116376372 A CN116376372 A CN 116376372A
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- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims description 52
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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
- C09D127/00—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 a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/16—Homopolymers or copolymers of vinylidene fluoride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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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
- C09D127/00—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 a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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
- C09D5/08—Anti-corrosive paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Non-Metallic Protective Coatings For Printed Circuits (AREA)
Abstract
The invention provides a printed circuit board surface super-hydrophobic treatment composite material and a preparation and use method thereof, wherein the printed circuit board surface super-hydrophobic treatment composite material comprises the following components: nano inorganic filler, pretreatment liquid, surfactant, organic solvent and diluent; the surface hydrophobicity modified composite material of the printed circuit board can form a protective layer with excellent wear resistance and superhydrophobicity on the surface of the printed circuit board, so that the mechanical damage protection and moisture absorption resistance improvement of the electronic circuit on the surface of the printed circuit board are realized, and the problem that the hygroscopicity of the existing printed circuit board base material influences the environmental stability of the printed circuit board is solved. The technology has the advantages of convenient operation, low cost, high efficiency and the like, has better compatibility with the prior art, and has low popularization and application cost.
Description
Technical Field
The invention relates to the technical field of material surface hydrophobicity modification, in particular to a printed circuit board surface super-hydrophobic treatment composite material and a preparation and use method thereof.
Background
Printed circuit boards are widely used in the automotive industry, aerospace, navigation, medical and consumer electronics, etc., as a core component for carrying and electrically interconnecting electronic components, known as the "parent of electronic products". The special application scene puts stringent requirements on the working stability and the signal transmission reliability of the printed circuit board, such as high-humidity and high-heat working environments like mines and coasts, in which the corrosion rate of copper on the surface of the printed circuit board can be accelerated, and the electrical interconnection quality and the signal transmission reliability of electronic circuits on the surface of the printed circuit board can be reduced due to factors such as moisture absorption of the substrate material on the surface of the circuit board, thereby reducing the working stability and the service life of an electronic system. Therefore, in the process of printed circuit board, it is important to improve the moisture-proof capability of the surface of the printed circuit board.
At present, the general method for improving the moisture-proof capability of the printed circuit board in the printed circuit board manufacturing industry is to coat three-proofing paint on the surface of the printed circuit board, and the technology realizes the improvement of the waterproof performance of electronic circuits and carried components thereof in the printed circuit board by means of the protective coating with the curing performance of the three-proofing paint. For example, xue Mingshan (CN 202010965917.0) of Guangdong Siquan new material stock discloses a preparation method of an ultraviolet aging resistant waterproof coating of a printed circuit board, which is used for improving the ultraviolet resistance and the waterproof performance of the printed circuit board and improving the environmental stability of the electrical performance of the printed circuit board. According to the functional components of the three-proofing paint, the three-proofing paint used in the current printed circuit board manufacturing field can be divided into four types of acrylic acid type, epoxy resin type, polyurethane type and organosilicon type, and the three-proofing paint has the characteristics of mature use process, low technical requirements and the like, but the paint is used in practice, and the high polymer material (protective layer) formed after the paint is solidified has certain moisture absorption performance, and the printed circuit board still has the problems of reduced electrical performance stability and the like after long-time use in high-humidity and high-temperature environments. In addition, most of the three-proofing paints at present mostly adopt benzene-containing substances (aromatic hydrocarbons) with high toxicity and the like as solvents, diluents and the like, and do not accord with the concept of green development at present. Therefore, the development of the printed circuit board surface hydrophobicity technology with excellent performance has important application value.
The main principle of the method for improving the surface hydrophobicity of the material by modifying the surface of the material is to utilize the action of a surfactant on the surface of the material, reduce the hydrophilic surface energy, water absorption and the like of the material, reduce the contact area of water and a coating and the residence time on the coating, thereby improving the moistureproof capacity of the material or the device. For example, the zodiac army et al (publication number CN101638785 a) of the scientific and technological limited company of the guangdong, proposed a method of adjusting the surface hydrophobicity of a printed circuit board by using carboxylate and the like through an OSP process, but the high temperature resistance of an organic film layer is poor; in the preparation of an anti-electromagnetic interference printed circuit board, shen Haiyan (CN 213342806U) of Dai-Tech Co., ltd.in Shenzhen, a method for preparing a waterproof coating layer by adopting Sol-Gel is proposed, a waterproof, dampproof and anti-corrosion net is formed on the surface, the net consists of ultrafine nano particles and has a certain gap, the heat dissipation performance of the outer surface layer of a main board and components is improved, when external water enters the device and drops on the printed circuit board, the external water is blocked by two layers of coatings, flows on the surface of the printed circuit board, and finally flows into a heat dissipation hole and is adsorbed by absorbent cotton in an absorbent tank, so that the overall waterproof of the printed circuit board is realized; special materials for spaceflight and Dong Heng et al (CN 110218102A and CN 115304404A) from technical institute of technology based on quartz fiber reinforced radome wave-transmitting complexSynthetic material substrate, invent hydrophobic SiO 2f /SiO 2 Wave-transparent material and SiO 2f /SiO 2 A composite material hydrophobic coating and a preparation method thereof; a super-hydrophobic nano composite material coating with excellent mechanical stability and a preparation method thereof are proposed by the university of Harbin industry, salty and noble force (CN 114686076A), a two-dimensional hydrophobic structure with a top film and a bottom film combined is adopted, the bonding force with a matrix is improved by an epoxy resin film layer on the bottom film, and the formed coating belongs to a non-uniform structure; henan university of science and technology Peng Shuge et al (CN 110117430B) propose a metal material substrate-based composite material with a superhydrophobic coating and a preparation method thereof, a substrate material and a preparation method thereof; the Beijing university of chemical industry Hong Tianyi discusses the theoretical basis of adopting a surfactant to adjust the surface hydrophobicity of a printed circuit board substrate in the research of complete pore liquid compounding of a circuit board based on quantum chemistry calculation. These studies have all solved specific technical problems in the application field, but the application in the printed circuit board field still has a certain bottleneck technical problem. As is well known, a printed circuit board is generally formed by manufacturing copper electronic circuits on the surface of an insulating substrate, and the surface of the printed circuit board is provided with an exposed area of an organic substrate material and an exposed area of a copper wire, so that the property difference of different materials increases the difficulty of realizing a superhydrophobic surface through surface modification under the condition that the electrical performance of the printed circuit board is not influenced. In view of the technical problems of the existing PCB surface hydrophobicity treatment materials and technologies, the inventor provides a composite material with the surface modified by super-hydrophobicity of a printed circuit and a use method thereof based on the technical methods of material surface grafting technology, nano effect and the like. The hydrophobic material can form a layer of uniform hydrophobic layer on the surface of the printed circuit board, the coating medium layer and the printed circuit board not only have excellent binding force, but also have excellent thermal stability and insulating property, and the problems of high hygroscopicity, poor durability and the like of the protective layer manufactured by adopting the three-oil-proof paint, OPS technology and the like in the prior art are overcome, so that the technical problems of environmental suitability and the like of the printed circuit board are further influenced. In addition, the hydrophobic coating manufacturing process provided by the inventor has excellent compatibility with the prior art process, and can be used on the prior production lineRealizing seamless butt joint and popularization and application.
Disclosure of Invention
Aiming at the problems that the prior printed circuit board surface protection technology has certain moisture absorption (such as RF-4 substrate-0.09 percent, PI substrate-0.7 percent and the like) due to the existence of an organic material substrate, an ink curing medium and the like, and further has adverse effects on the stability of the electrical performance of the printed circuit board, the service life of electronic products and the like, the invention provides a modified inorganic nanoparticle filled composite printed circuit board surface super-hydrophobic coating material, a preparation method and a use method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a preparation method of a printed circuit board surface super-hydrophobic treatment composite material comprises the following steps:
step 1: hydrophobic treatment of nano inorganic filler; the inorganic nano-filler is placed into the pretreatment liquid at 20-25 ℃ for presoaking for 24-48 hours, and the mass concentration of the inorganic nano-filler in the pretreatment liquid is 10-20 g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: 2-5 vol% of surfactant, 55-85 vol% of organic solvent and 13-40 vol% of diluent in the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 50-65 ℃ for ultrasonic treatment for 30-60 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 30-60 g/L; maintaining the temperature of the system at 50-65 ℃, heating and stirring for 30-45 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
Preferably, the particle size of the inorganic nano filler is 10-200 nm, and the inorganic nano filler is at least one selected from nano zinc oxide powder, nano titanium dioxide powder, nano silicon dioxide powder, nano calcium carbonate powder and nano aluminum oxide powder.
Preferably, the surfactant is selected from: at least one of trimethoxy (1H, 2H-tridecafluoron-octyl) silane, polytetrafluoroethylene, methyltriethoxysilane or polydimethylsiloxane.
Preferably, the polymer is selected from: at least one of polyvinylidene fluoride, polytetrafluoroethylene or polydimethylsiloxane.
Preferably, the organic solvent is selected from: n, N-dimethylacetamide, N, N-dimethylformamide, N-methylpyrrolidone or dimethylsulfoxide.
Preferably, the diluent is selected from: at least one of absolute ethanol, butanol, methanol, carbon tetrachloride, acetone or ethylene glycol.
The invention also provides the printed circuit board surface super-hydrophobic treatment composite material obtained by the preparation method.
The invention also provides a using method of the printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
(1) Cleaning the printed circuit board to be treated in a cleaning solution, and drying;
(2) Then coating the printed circuit board surface super-hydrophobic treatment composite material obtained in the claim 7 on the printed circuit board surface;
(3) The coated printed circuit board is put into an oven for curing at the temperature of 110-130 ℃ for 5-15 minutes,
(4) Washing with tap water, and drying in an oven at 110-130 ℃ to obtain the product.
Preferably, the method for coating the surface of the printed board in the step (2) with the super-hydrophobic coating material is selected from the following steps: spin coating, silk screen printing, spray coating, dip coating, and ink jet printing.
The nano inorganic filler is subjected to hydrophobic treatment to form a super-hydrophobic medium, and certain roughness and hydrophobicity are provided on the surface of the printed circuit board, so that micro water drops formed by moisture absorption can realize the transition from a Wenzel state to a Cassie state on the surface.
The added surfactant has the performances of modifying the filler, the surface of the printed circuit board and the like through surface grafting, and the physical and chemical bridging effect formed between different surfaces of the surfactant enhances the direct binding force between the coating and the substrate and the binding force inside the coating, thereby improving the durability of the coating.
The function of the diluent is mainly to regulate and control the viscosity of the composite coating material and improve the process operability of the composite coating material.
The main function of the added polymer is to form a backbone network structure of the hydrophobic medium layer, so that the adhesive force between the medium layer and the substrate material can be increased, and the mechanical properties (such as wear resistance) and the like are enhanced.
The main function of the organic solvent is to dissolve the polymer added into the composite material system, so that the modified nano particles and the organic polymer form a uniform liquid system, and the film forming effect is facilitated.
Compared with the prior art, the invention has the following beneficial effects:
based on the basic principle of hydrophobic modification of the material surface, the inventor provides a novel composite material for modifying the surface of a printed circuit board and a use method thereof, adopts a single composite material to treat the printed circuit board, and obtains excellent binding force and hydrophobic treatment effect on the surface (copper electronic circuit and substrate) with multiple material characteristics. The technology is ingenious in that the material hydrophobicity treatment and the surface protection are organically combined, the problem of hygroscopicity of the existing printed circuit board base material is solved on the premise of realizing the surface protection of the printed circuit board, and the application performance (such as the service life and the like) of the printed circuit board in severe environments such as high humidity and the like is improved. The inventor adopts amphiphilic surface activity to graft hydrophobic treatment on the surfaces of nano inorganic filler particles, so that not only can hydrophobic functional units be formed, but also the binding force between the particles and the network structure polymer and the binding force between the hydrophobic medium layer and the substrate are improved, and the hydrophobic medium layer has good mechanical property and durability.
The invention realizes the excellent waterproof performance of the surface of the printed circuit board, and the hydrophobic coating is very stable, thereby being beneficial to realizing the application extension of the printed circuit board under severe environment, the compromise of corrosion resistance of products and the guarantee of high-frequency signal transmission quality, and the like. The technology has the advantages of convenient operation, low cost, high efficiency and the like, has better compatibility with the prior art, has low technical upgrading cost and controllable risk for enterprises, and improves the capability of the printed circuit board product for coping with challenges brought by severe environments.
Drawings
Fig. 1 is a graph of contact angle measurements of a superhydrophobic coating prepared on a printed circuit board using the method of the invention, the contact angle being 146.2 °.
Fig. 2 is an SEM test chart (magnification 80000) of a superhydrophobic coating prepared on a printed circuit board using the method of the present invention.
Fig. 3 is a graph of contact angle measurements of a superhydrophobic coating prepared on a printed circuit board using the method of the invention, the contact angle being 116.2 °.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Example 1
The embodiment provides a preparation method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
step 1: hydrophobic treatment of nano inorganic filler; the inorganic nano-filler is placed into a pretreatment liquid at 20 ℃ for presoaking for 24 hours, and the mass concentration of the inorganic nano-filler in the pretreatment liquid is 10g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: surfactant with the volume percentage concentration of 5vol%, organic solvent with the volume percentage concentration of 55vol% and diluent with the volume percentage concentration of 40vol% in the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 50 ℃ for ultrasonic treatment for 30 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 30g/L; maintaining the temperature of the system at 50 ℃, heating and stirring for 30 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
In this embodiment, the particle size of the inorganic nano filler is 10-200 nm, and is selected from nano zinc oxide powder.
In this embodiment, the surfactant is selected from: trimethoxy (1H, 2H-tridecafluoron-octyl) silane;
in this embodiment, the polymer is selected from: polyvinylidene fluoride;
in this embodiment, the organic solvent is selected from: n, N-dimethylacetamide;
in this embodiment, the diluent is selected from the group consisting of: absolute ethyl alcohol.
The nano inorganic filler is subjected to hydrophobic treatment to form a super-hydrophobic medium, and certain roughness and hydrophobicity are provided on the surface of the printed circuit board, so that micro water drops formed by moisture absorption can realize the transition from a Wenzel state to a Cassie state on the surface.
The added surfactant has the performances of modifying the filler, the surface of the printed circuit board and the like through surface grafting, and the physical and chemical bridging effect formed between different surfaces of the surfactant enhances the direct binding force between the coating and the substrate and the binding force inside the coating, thereby improving the durability of the coating.
The function of the diluent is mainly to regulate and control the viscosity of the composite coating material and improve the process operability of the composite coating material.
The main function of the added polymer is to form a backbone network structure of the hydrophobic medium layer, so that the adhesive force between the medium layer and the substrate material can be increased, and the mechanical properties (such as wear resistance) and the like are enhanced.
The main function of the organic solvent is to dissolve the polymer added into the composite material system, so that the modified nano particles and the organic polymer form a uniform liquid system, and the film forming effect is facilitated.
Example 2
The embodiment provides a preparation method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
step 1: hydrophobic treatment of nano inorganic filler; placing inorganic nano-filler into the pretreatment liquid at 25 ℃ for presoaking for 48 hours, wherein the mass concentration of the inorganic nano-filler in the pretreatment liquid is 20g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: surfactant with the volume percentage concentration of 2vol%, organic solvent with the volume percentage concentration of 85vol% and diluent with the volume percentage concentration of 13vol% of the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 65 ℃ for ultrasonic treatment for 60 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 60g/L; maintaining the system temperature at 65 ℃, heating and stirring for 45 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
In this embodiment, the particle size of the inorganic nanofiller is 200nm and is selected from nano titanium dioxide powder.
In this embodiment, the surfactant is selected from: polytetrafluoroethylene;
in this embodiment, the polymer is selected from: polytetrafluoroethylene.
In this embodiment, the organic solvent is selected from: n, N-dimethylformamide;
in this embodiment, the diluent is selected from the group consisting of: butanol.
Example 3
The embodiment provides a preparation method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
step 1: hydrophobic treatment of nano inorganic filler; placing inorganic nano-filler into a pretreatment liquid at 22 ℃ for presoaking for 30 hours, wherein the mass concentration of the inorganic nano-filler in the pretreatment liquid is 13g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: surfactant with the volume percentage concentration of 5vol%, organic solvent with the volume percentage concentration of 65vol% and diluent with the volume percentage concentration of 30vol% in the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 55 ℃ for ultrasonic treatment for 40 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 40g/L; maintaining the temperature of the system at 55 ℃, heating and stirring for 35 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
In this embodiment, the particle size of the inorganic nanofiller is 10 to 200nm and is selected from the group consisting of nano silica powder.
In this embodiment, the surfactant is selected from: methyltriethoxysilane.
In this embodiment, the polymer is selected from: polydimethyl siloxane.
In this embodiment, the organic solvent is selected from: n-methylpyrrolidone.
In this embodiment, the diluent is selected from the group consisting of: carbon tetrachloride.
Example 4
The embodiment provides a preparation method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
step 1: hydrophobic treatment of nano inorganic filler; placing inorganic nano-filler into the pretreatment liquid at 23 ℃ for presoaking for 40 hours, wherein the mass concentration of the inorganic nano-filler in the pretreatment liquid is 15g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: surfactant with the volume percentage concentration of 5vol%, organic solvent with the volume percentage concentration of 75vol% and diluent with the volume percentage concentration of 20vol% in the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 60 ℃ for ultrasonic treatment for 50 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 50g/L; maintaining the system temperature at 60 ℃, heating and stirring for 40 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
In this embodiment, the particle size of the inorganic nano filler is 10-200 nm, and the inorganic nano filler is nano calcium carbonate powder and nano alumina powder.
In this embodiment, the surfactant is selected from: methyltriethoxysilane and polydimethylsiloxane.
In this embodiment, the polymer is selected from: polyvinylidene fluoride and polytetrafluoroethylene.
In this embodiment, the organic solvent is selected from: n, N-dimethylacetamide and dimethylsulfoxide.
In this embodiment, the diluent is: acetone and ethylene glycol.
Example 5
The embodiment provides a preparation method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
step 1: hydrophobic treatment of nano inorganic filler; placing inorganic nano-filler into 24 ℃ pretreatment liquid for presoaking for 43 hours, wherein the mass concentration of the inorganic nano-filler in the pretreatment liquid is 17g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: surfactant with the volume percentage concentration of 4vol%, organic solvent with the volume percentage concentration of 76vol% and diluent with the volume percentage concentration of 20vol% in the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 62 ℃ for ultrasonic treatment for 55 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 55g/L; maintaining the system temperature at 63 ℃, heating and stirring for 42 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
In this embodiment, the particle size of the inorganic nanofiller is 10-200 nm and is selected from nano alumina powder.
In this embodiment, the surfactant is selected from: trimethoxy (1H, 2H-tridecafluoron-octyl) silane, and at least one of methyltriethoxysilane and polydimethylsiloxane.
In this embodiment, the polymer is: polyvinylidene fluoride, polytetrafluoroethylene, and polydimethylsiloxane.
In this embodiment, the organic solvent is: n, N-dimethylacetamide, N, N-dimethylformamide, N-methylpyrrolidone.
In this embodiment, the diluent is: methanol, carbon tetrachloride, ethylene glycol.
Example 6
The embodiment provides a preparation method and a use method of a printed circuit board surface super-hydrophobic treatment composite material, comprising the following steps:
(1) Printed circuit board pretreatment
The basic process flow is as follows: cutting a copper-clad plate with the copper layer thickness of 12 mu m into a 40mm multiplied by 40mm template by a plate cutting machine, cleaning by tap water, cleaning by acid cleaning liquid (60 seconds, 32 ℃), cleaning by alkaline cleaning liquid (60 seconds, 55 ℃), cleaning by tap water and drying by hot air;
the formula of the acidic cleaning liquid comprises the following components: 5.0% dilute sulfuric acid solution;
the alkaline cleaning solution comprises the following formula: 5.0% sodium carbonate, 1.5% sodium bicarbonate, 2.0% sodium stearyl benzene sulfonate;
(2) Modification of nanosilica
The process flow comprises the following steps: adding 25g of 15nm silicon dioxide into 300ml of modified treatment liquid, stirring for 48 hours, centrifuging, adding ethanol, ultrasonically cleaning for three times, filtering, and drying in an oven at 80 ℃ for 5 hours;
nano SiO 2 Preparing a modification treatment liquid: 2.5g of trimethoxytridecafluoron-octyl silane and 300ml of absolute ethyl alcohol are respectively measured,mixing under continuous stirring, wherein the addition sequence of the components is as follows: trimethoxytridecafluoron-octyl silane- & gt absolute ethyl alcohol to finish preparation;
(3) The preparation of the hydrophobic treatment composite material of the printed circuit board comprises the following steps: adding 0.3g of hydrophobic treated nano silicon dioxide into 20ml of N, N-dimethylacetamide, carrying out ultrasonic dispersion treatment for 1 hour, adding 0.80g of polyvinylidene fluoride, heating and stirring at 60 ℃ for 30 minutes, stopping heating, and stirring until the composite material is cooled to room temperature;
(4) The hydrophobic treatment of the printed circuit board comprises the following process flows: placing the pretreated printed circuit board on a workbench of a spin coater, coating the super-hydrophobic composite material on the surface of the printed circuit board, dripping the super-hydrophobic composite material on the surface of the printed circuit board, spin-coating the composite material for 15s (the rotating speed of a rotating table is 1500 rpm), placing the printed circuit board coated with the material into a baking oven for curing (the curing temperature is 120 ℃ for 5-15 minutes), washing with tap water, and drying in the baking oven at the temperature of 120 ℃ to obtain a product;
(5) Surface modified printed circuit board performance test
(a) Contact angle test: the hydrophobic coating was subjected to a contact angle test, the contact angle photograph is shown in fig. 1, and the contact angle is measured to be 146.2 degrees;
(b) SEM test: SEM testing was performed on the hydrophobic coating and the test results are shown in fig. 2.
Example 7
The embodiment provides a preparation method and a use method of a printed circuit board surface super-hydrophobic treatment composite material, comprising the following steps:
(1) Printed circuit board pretreatment
The basic process flow is as follows: cutting a copper-clad plate with the copper layer thickness of 12 mu m into a 40mm multiplied by 40mm template by using a plate cutting machine, cleaning with tap water, cleaning with an acid cleaning solution (60 seconds, 32 ℃), cleaning with tap water, cleaning with an alkaline cleaning solution (60 seconds, 55 ℃), cleaning with tap water and drying with hot air;
the formula of the acidic cleaning liquid comprises the following components: 5.0% dilute sulfuric acid solution;
the alkaline cleaning solution comprises the following formula: 5.0% sodium carbonate, 1.5% sodium bicarbonate, 2.0% sodium stearyl benzene sulfonate;
(2) Modification of nano zinc oxide
The process flow comprises the following steps: 25g of 15nm zinc oxide is added into 300ml of modified treatment liquid, stirred for 48 hours, centrifuged, ultrasonically cleaned by adding ethanol for three times, filtered and dried in an oven at 80 ℃ for 5 hours;
preparing nano ZnO modified treatment liquid: 2.5g of trimethoxytridecafluoron-octyl silane, 250ml of acetone and 50ml of dimethyl sulfoxide are respectively measured and mixed under continuous stirring, and the addition sequence of the components is as follows: trimethoxytridecafluoron-octyl silane-dimethyl sulfoxide-acetone to complete the preparation;
(3) The preparation of the hydrophobic treatment composite material of the printed circuit board comprises the following steps: adding 0.25g of nano zinc oxide subjected to hydrophobic treatment into 25ml of dimethyl sulfoxide, carrying out ultrasonic dispersion treatment for 1 hour, adding 0.75g of polyvinylidene fluoride, heating and stirring at 60 ℃ for 30 minutes, stopping heating, and stirring until the composite material is cooled to room temperature;
(4) The hydrophobic treatment of the printed circuit board comprises the following process flows: placing the pretreated printed circuit board on a workbench of a spin coater, coating the super-hydrophobic composite material on the surface of the printed circuit board, dripping the super-hydrophobic composite material on the surface of the printed circuit board, spin-coating the composite material for 15s (the rotating speed of a rotating table is 1500 rpm), placing the printed circuit board coated with the material into a baking oven for curing (the curing temperature is 120 ℃ for 5-15 minutes), washing with tap water, and drying in the baking oven at the temperature of 120 ℃ to obtain a product;
(5) Surface modified printed circuit board performance test
Contact angle test: the hydrophobic coating was subjected to a contact angle test, the photograph of which is shown in fig. 3, and the contact angle was measured to be 116.2 °.
Example 8
The embodiment provides a using method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
(1) Cleaning the printed circuit board to be treated in a cleaning solution, and drying;
(2) Then coating the surface of the printed board with the printed circuit board surface superhydrophobic treatment composite material obtained in one of the embodiments 1-5;
(3) The coated printed circuit board is put into an oven for curing at 110 ℃ for 5 minutes,
(4) Washing with tap water, and drying in an oven at 110 ℃ to obtain the product.
The method for coating the super-hydrophobic coating material on the surface of the printed board in the step (2) is spin coating.
Example 9
The embodiment provides a using method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
(1) Cleaning the printed circuit board to be treated in a cleaning solution, and drying;
(2) Then coating the surface of the printed board with the printed circuit board surface superhydrophobic treatment composite material obtained in one of the embodiments 1-5;
(3) The coated printed circuit board is put into an oven for curing at 130 ℃ for 15 minutes,
(4) Washing with tap water, and drying in an oven at 130 ℃ to obtain the product.
Preferably, the method for coating the super-hydrophobic coating material on the surface of the printed board in the step (2) is silk screen printing.
Example 10
The embodiment provides a using method of a printed circuit board surface super-hydrophobic treatment composite material, which comprises the following steps:
(1) Cleaning the printed circuit board to be treated in a cleaning solution, and drying;
(2) Then coating the surface of the printed board with the printed circuit board surface superhydrophobic treatment composite material obtained in one of the embodiments 1-5;
(3) The coated printed circuit board is put into an oven for curing at 120 ℃ for 10 minutes,
(4) Washing with tap water, and drying in an oven at 120 ℃ to obtain the product.
Preferably, the method for coating the surface of the printed board in the step (2) with the super-hydrophobic coating material is selected from the following steps: one of spray coating, dip coating, and ink jet printing.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims of this invention, which are within the skill of those skilled in the art, can be made without departing from the spirit and scope of the invention disclosed herein.
Claims (9)
1. The preparation method of the super-hydrophobic treatment composite material on the surface of the printed circuit board is characterized by comprising the following steps of:
step 1: hydrophobic treatment of nano inorganic filler; the inorganic nano-filler is placed into the pretreatment liquid at 20-25 ℃ for presoaking for 24-48 hours, and the mass concentration of the inorganic nano-filler in the pretreatment liquid is 10-20 g/L; then centrifugal separation, ultrasonic treatment and washing are carried out, the treatment is repeated for three times, and finally, the hydrophobic inorganic nano filler is obtained after drying; the pretreatment liquid comprises: 2-5 vol% of surfactant, 55-85 vol% of organic solvent and 13-40 vol% of diluent in the pretreatment liquid;
step 2: preparing a composite material subjected to surface super-hydrophobic treatment of a printed circuit board; placing the hydrophobic inorganic nano filler obtained in the step 1 into an organic solvent with the temperature of 50-65 ℃ for ultrasonic treatment for 30-60 minutes, and then adding a polymer into the organic solvent under the state of continuous stirring, wherein the mass concentration of the polymer in the organic solvent is 30-60 g/L; maintaining the temperature of the system at 50-65 ℃, heating and stirring for 30-45 minutes, and finally cooling to room temperature to obtain the super-hydrophobic coating material on the surface of the printed circuit board.
2. The method for preparing the printed circuit board surface super-hydrophobic treatment composite material according to claim 1, which is characterized in that: the particle size of the inorganic nano filler is 10-200 nm, and the inorganic nano filler is at least one selected from nano zinc oxide powder, nano titanium dioxide powder, nano silicon dioxide powder, nano calcium carbonate powder or nano aluminum oxide powder.
3. The method for preparing the printed circuit board surface super-hydrophobic treatment composite material according to claim 1, which is characterized in that: the surfactant is selected from the group consisting of: at least one of trimethoxy (1H, 2H-tridecafluoron-octyl) silane, polytetrafluoroethylene, methyltriethoxysilane or polydimethylsiloxane.
4. The method for preparing the printed circuit board surface super-hydrophobic treatment composite material according to claim 1, which is characterized in that: the polymer is selected from: at least one of polyvinylidene fluoride, polytetrafluoroethylene or polydimethylsiloxane.
5. The method for preparing the printed circuit board surface super-hydrophobic treatment composite material according to claim 1, which is characterized in that: the organic solvent is selected from the group consisting of: n, N-dimethylacetamide, N, N-dimethylformamide, N-methylpyrrolidone or dimethylsulfoxide.
6. The method for preparing the printed circuit board surface super-hydrophobic treatment composite material according to claim 1, which is characterized in that: the diluent is selected from: at least one of absolute ethanol, butanol, methanol, carbon tetrachloride, acetone or ethylene glycol.
7. The printed circuit board surface superhydrophobic treatment composite material obtained by the preparation method according to any one of claims 1 to 6.
8. The method for using the printed circuit board surface super-hydrophobic treatment composite material according to claim 7, which is characterized by comprising the following steps:
(1) Cleaning the printed circuit board to be treated in a cleaning solution, and drying;
(2) Then coating the printed circuit board surface super-hydrophobic treatment composite material obtained in the claim 7 on the printed circuit board surface;
(3) The coated printed circuit board is put into an oven for curing at the temperature of 110-130 ℃ for 5-15 minutes,
(4) Washing with tap water, and drying in an oven at 110-130 ℃ to obtain the product.
9. The method for using the printed circuit board surface super-hydrophobic treatment composite material according to claim 8, wherein the method comprises the following steps: the method for coating the super-hydrophobic coating material on the surface of the printed board in the step (2) is selected from the following steps: spin coating, silk screen printing, spray coating, dip coating, and ink jet printing.
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| CN116120808A (en) * | 2023-01-03 | 2023-05-16 | 国家石油天然气管网集团有限公司 | Durable super-hydrophobic anti-corrosion coating and preparation method thereof |
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| CN109575769A (en) * | 2018-10-30 | 2019-04-05 | 天津大学 | Super-hydrophobic and super oleophobic coating of one kind and preparation method thereof |
| CN111138917A (en) * | 2020-01-17 | 2020-05-12 | 中北大学 | Preparation method of super-hydrophobic coating based on micro/nano inorganic particle synergistic enhanced fluorocarbon resin |
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