CN111647354A - Waterproof heat-conducting coating and preparation method thereof - Google Patents

Waterproof heat-conducting coating and preparation method thereof Download PDF

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CN111647354A
CN111647354A CN202010616288.0A CN202010616288A CN111647354A CN 111647354 A CN111647354 A CN 111647354A CN 202010616288 A CN202010616288 A CN 202010616288A CN 111647354 A CN111647354 A CN 111647354A
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waterproof heat
conducting coating
conducting
waterproof
heat
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刘伟
付冲
杨高
梁坚伟
黄梅鹏
曾宝宝
林景辉
范国威
冯汉铧
谢文漾
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Guangdong University of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D183/00Coating 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
    • C09D183/04Polysiloxanes
    • C09D183/08Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

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Abstract

The invention discloses a waterproof heat-conducting coating and a preparation method thereof, wherein the waterproof heat-conducting coating provided by the invention adopts a preparation method of combining glue and powder, fluorinated resin is selected as the glue to play a role in bonding nanoscale hydrophobic silicon dioxide and few layers of boron nitride, the nanoscale hydrophobic silicon dioxide is used as hydrophobic powder to generate a nanometer rough structure on the surface of the coating, and few layers of boron nitride are used as a reinforcing phase to play a role in enhancing heat conduction. The waterproof heat-conducting coating is sprayed on an electronic product to form a waterproof heat-conducting coating, and the detection shows that the contact angle of the waterproof heat-conducting coating is more than 120 degrees, and the heat-conducting property is obviously improved. The waterproof heat-conducting coating sprayed on the electronic product not only has the traditional three-proofing paint function, but also has good heat-conducting property and waterproof property, can solve the problems of heat dissipation and water resistance of the existing electronic product, and has wide application prospect in the electronic industry.

Description

Waterproof heat-conducting coating and preparation method thereof
Technical Field
The invention relates to the field of coatings, in particular to a waterproof heat-conducting coating and a preparation method of the waterproof heat-conducting coating.
Background
In the use and storage process of electronic products, the electronic products usually need to be subjected to chemical, vibration, high-dust, salt mist, moisture and high-temperature environments, and the problems of corrosion, softening, deformation, mildew and the like of circuit boards and electronic components of the circuit boards can occur, so that the faults are caused. In order to make the printed circuit board of the electronic product have good three-proofing protection capability, the printed circuit board is usually sprayed with a three-proofing protection coating after debugging.
According to the American military standard MIL-I-46058C, the three-proofing paint is mainly divided into five major products such as acrylic resin, epoxy resin, organic silicon resin, polyurethane, parylene and the like from the chemical composition. Three-proofing paint in the traditional sense has obvious effects on moisture resistance and dust resistance, but is still unsatisfactory on other functions, such as waterproof performance and heat-conducting performance. Electronic products such as mobile phones have become an indispensable role in daily life along with the development of intellectualization, and mobile phones and the like fall into water due to some unexpected reasons in life, so that once water enters, irreparable loss is caused to users. Electronic products can generate heat in the use process, and the user experience can be influenced by overheating of the electronic products.
At present, waterproof and moistureproof treatment and heat dissipation treatment of electronic product equipment are mostly carried out through structural design, for example, seams of a shell are protected by rubber gaskets, ventilation holes are designed on the shell for heat dissipation, and the like, and the problems cannot be fundamentally solved by the treatment method.
Chinese patent CN201610624207.5 describes a method for preparing a circuit board with a super-hydrophobic waterproof nano-coating, comprising the following steps: s1, preparing the super-hydrophobic waterproof nano paint: the method comprises the following substeps: s1-1, preparing materials: the components are prepared according to the following parts by weight: 5-6 parts of organic-inorganic hybrid nano resin, 1-30 parts of nano-scale silica sol, 0.1-10 parts of super-hydrophobic silica, 1-10 parts of isopropanol and 30-70 parts of water; s1-2, mixing and stirring; s2, spraying; and S3, detecting. This patent can promote the waterproof performance of circuit board, nevertheless can't solve the heat dissipation problem of circuit board.
Disclosure of Invention
The invention provides a waterproof heat-conducting coating and a preparation method of the waterproof heat-conducting coating.
In order to achieve the purpose, the invention adopts the following technical scheme:
the waterproof heat-conducting coating comprises the following components in parts by weight:
6-8 parts of fluorinated resin, 1-3 parts of nanoscale hydrophobic silicon dioxide, 1-3 parts of few-layer boron nitride and 200-500 parts of organic solvent.
Optionally, the fluorinated resin is any one of fluorine-modified organosilane, fluorinated epoxy resin, organic silicon polymer resin and silicon fluorine resin.
Optionally, the organic solvent comprises one or more of ethyl acetoacetate, ethyl acetate and ethanol.
A preparation method of a waterproof heat-conducting coating comprises the following steps:
s11, preparing the following components in parts by weight: 6-8 parts of fluorinated resin, 1-3 parts of nanoscale hydrophobic silicon dioxide, 1-3 parts of few-layer boron nitride and 200-500 parts of organic solvent;
s12, stirring and mixing the components prepared in the step S11 at a high speed to obtain the waterproof heat-conducting coating.
Optionally, the stirring speed of the high-speed stirring in the step S12 is 1300-1700 rpm, and the stirring time is 5-10 min;
the few-layer boron nitride is prepared by the following steps:
mixing single-layer boron nitride with sodium hypochlorite to form mixed slurry, carrying out ball milling on the mixed slurry, and then centrifuging to obtain a lower-layer product;
sequentially cleaning, filtering and drying the lower-layer product to obtain solid particles;
dispersing the solid particles in isopropanol for ultrasonic treatment, and centrifuging to obtain an upper-layer mixed solution;
and filtering and drying the upper layer mixed solution to obtain the few-layer boron nitride.
Optionally, when the single-layer boron nitride and the sodium hypochlorite are mixed to form the mixed slurry, the mass ratio of the single-layer boron nitride to the sodium hypochlorite is 1: 50;
when the mixed slurry is subjected to ball milling, the ball milling rotation speed is 150rpm, and the ball milling time is 16 h;
when the lower-layer product is obtained by the centrifugation, the centrifugation rotating speed is 5000rpm, and the centrifugation time is 10 min.
Optionally, the lower-layer product is sequentially washed, filtered and dried to obtain solid particles, and the method specifically includes:
sequentially cleaning the lower-layer product by using three solutions of hydrochloric acid, water and ethanol to obtain a neutral mixed solution;
carrying out suction filtration on the neutral mixed solution by using a filter membrane with the specification of 1.5-2.5 microns to obtain a solid product;
drying the solid product to obtain solid particles.
Optionally, when the solid particles are dispersed in isopropanol and subjected to ultrasound, the ratio of the solid particles to the isopropanol is 0.5mg/mL, and the ultrasound time is 0.5 h;
when the upper-layer mixed solution is obtained through centrifugation, the centrifugation rotating speed is 3000rpm, and the centrifugation time is 30 min;
and when the upper-layer mixed solution is filtered and dried, the specification of the filtering membrane is 1.5-2.5 mu m.
A preparation method of a waterproof heat-conducting coating comprises the following steps: the waterproof heat-conducting coating or the waterproof heat-conducting coating prepared by the preparation method is sprayed on the electronic component through a spraying process to form the waterproof heat-conducting coating.
Optionally, the thickness of the waterproof heat-conducting coating is 1-2 μm;
the waterproof heat-conducting coating is sprayed on the electronic component through a spraying process, and then the method further comprises the following steps:
and baking the electronic part sprayed with the waterproof heat-conducting coating for 1-3 hours at 50-70 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the waterproof heat-conducting coating provided by the invention adopts a preparation method of combining glue and powder. The fluorinated resin is selected as glue to bond the nanoscale hydrophobic silicon dioxide and the few layers of boron nitride, the fluorinated resin can modify the surface of an object to form low surface chemical energy, the nanoscale hydrophobic silicon dioxide is used as hydrophobic powder to generate a nano rough structure on the surface of the coating, and the few layers of boron nitride is used as a reinforcing phase to reinforce the heat conduction effect. The waterproof heat-conducting coating is sprayed on an electronic product to form a waterproof heat-conducting coating, and the detection shows that the contact angle of the waterproof heat-conducting coating provided by the invention is more than 120 degrees, and the heat-conducting property is obviously improved. The waterproof heat-conducting coating sprayed on the electronic product not only has the traditional three-proofing paint function, but also has good heat-conducting property and waterproof property, can solve the problems of heat dissipation and water resistance of the existing electronic product, and has wide application prospect in the electronic industry.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a thermal imaging test chart of coatings prepared in examples 1-2 of the present invention and comparative example 1;
FIG. 2 is a thermal imaging test chart of the coatings prepared in comparative examples 2 to 4 of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The invention provides a waterproof heat-conducting coating which comprises the following components in parts by weight:
6-8 parts of fluorinated resin, 1-3 parts of nanoscale hydrophobic silicon dioxide, 1-3 parts of few-layer boron nitride and 200-500 parts of organic solvent.
The waterproof heat-conducting coating provided by the invention adopts a preparation method of combining glue and powder, wherein fluorinated resin is selected as the glue to play a role in bonding the nanoscale hydrophobic silicon dioxide and the few layers of boron nitride, the nanoscale hydrophobic silicon dioxide is used as the hydrophobic powder to generate a nanometer rough structure on the surface of the coating, and the few layers of boron nitride are used as a reinforcing phase to play a role in enhancing heat conduction, so that the coating has good waterproof heat-conducting property.
In the present invention, the fluorine-modified organosilane, the fluorinated epoxy resin, the silicone polymer resin, or the silicone fluorine resin is preferably a silicone fluorine resin.
The organic solvent comprises one or more of ethyl acetoacetate, ethyl acetate and ethanol, and more preferably ethyl acetoacetate.
The invention also provides a preparation method of the waterproof heat-conducting coating, which comprises the following steps:
s11, preparing the following components in parts by weight: 6-8 parts of fluorinated resin, 1-3 parts of nanoscale hydrophobic silicon dioxide, 1-3 parts of few-layer boron nitride and 200-500 parts of organic solvent;
s12, stirring and mixing the components prepared in the step S11 at a high speed to obtain the waterproof heat-conducting coating.
Wherein the stirring speed of the high-speed stirring in the step S12 is 1300-1700 rpm, and the stirring time is 5-10 min.
In a preferred embodiment of the invention, the few-layer boron nitride is prepared by the following steps:
s21, mixing single layer boron nitride with sodium hypochlorite at a ratio of 1: 50, ball milling and stripping for 16h at the room temperature and 150rpm in a ball mill;
s22, centrifuging the product obtained in the step S11 in a high-speed centrifuge at 5000rpm for 10min to obtain a lower-layer product;
s23, sequentially cleaning the lower-layer product obtained in the step 22 with three solutions of hydrochloric acid, water and ethanol to obtain a neutral mixed solution, performing suction filtration with a filter membrane with the specification of 1.5-2.5 microns to obtain a solid, and drying to obtain solid particles;
s24, dispersing the solid particles obtained in the step S23 in isopropanol at a speed of 0.5mg/mL for 0.5h by ultrasonic treatment, centrifuging at a speed of 3000rpm for 30min to obtain an upper white mixed liquid, and finally performing suction filtration and drying by using a filter membrane with a specification of 1.5-2.5 microns to obtain the few-layer boron nitride.
The invention also provides a preparation method of the waterproof heat-conducting coating, namely after the waterproof heat-conducting coating is prepared, the waterproof heat-conducting coating is sprayed on the electronic component through a spraying process, and then the electronic component is baked for 1-3 hours at 50-70 ℃ to obtain the waterproof heat-conducting coating. The thickness of the waterproof heat-conducting coating is 1-2 mu m, and the electronic component is preferably a circuit board.
According to the embodiment of the invention, the waterproof performance of the waterproof heat-conducting coating is tested through a contact angle test, the heat-conducting performance of the waterproof heat-conducting coating is tested through a thermal imaging test, and the test result shows that the waterproof heat-conducting coating has good heat-conducting performance and hydrophobic performance.
The waterproof heat-conducting coating prepared by the invention has the function of the traditional three-proofing paint, can protect electronic components from being corroded by the environment, further improves the reliability of the electronic components and prolongs the service life of the electronic components. Furthermore, the waterproof heat-conducting coating also has good heat-conducting performance and waterproof performance, and the ultrathin thickness ensures that the waterproof heat-conducting coating does not influence the normal work of the electronic component. The waterproof heat-conducting coating has excellent performance, is safe and environment-friendly, and has wide application prospect in the electronic industry.
The invention is further illustrated by the following specific examples. The starting materials used in the present invention are either commercially available or commonly used in the art, and the methods in the examples below are conventional in the art unless otherwise specified.
Example 1
In this embodiment 1, a waterproof heat-conducting coating is prepared, and the preparation and performance detection processes are as follows:
s1, preparing the waterproof heat-conducting paint, which specifically comprises the following substeps:
s1-1, preparing materials: the components are prepared according to the following parts by weight: 7 parts of silicon-fluorine resin, 2.1 parts of nano-scale hydrophobic silicon dioxide, 1.5 parts of few-layer boron nitride and 437.5 parts of ethyl acetoacetate;
s1-2, mixing and stirring: the components are uniformly mixed, poured into a high-speed stirrer, and stirred for 8min at the rotating speed of 1500r/min to obtain the waterproof heat-conducting coating.
S2, spraying: spraying waterproof heat-conducting paint with the spraying thickness of 1 micron on the silicon wafer by adopting a spraying process to obtain the silicon wafer with the waterproof heat-conducting coating; wherein the area of the silicon wafer is 1cm2
S3, detection:
s3-1: and (3) detecting the waterproof performance: a silicon wafer with a waterproof heat-conducting coating is used for carrying out contact angle test, and the result shows that the contact angle is more than 120 degrees; the water was dropped on the surface of the silicon wafer having the waterproof heat conductive coating, and it was observed that the shape thereof remained spherical and the surface of the coating was not wetted.
S3-2: and (3) detecting the heat conducting property: and (3) carrying out thermal imaging test on the silicon wafer with the waterproof heat-conducting coating on a thermal platform, and detecting the heat-conducting property of the silicon wafer.
Example 2
In this embodiment 2, a waterproof heat-conducting coating is prepared, and the preparation and performance detection processes are as follows:
s1, preparing the waterproof heat-conducting paint, which specifically comprises the following substeps:
s1-1, preparing materials: the components are prepared according to the following parts by weight: 7 parts of silicon-fluorine resin, 1.5 parts of nano-scale hydrophobic silicon dioxide, 2.1 parts of few-layer boron nitride and 437.5 parts of ethyl acetoacetate;
s1-2, mixing and stirring: the components are uniformly mixed, poured into a high-speed stirrer, and stirred for 8min at the rotating speed of 1500r/min to obtain the waterproof heat-conducting coating.
S2, spraying: spraying waterproof heat-conducting paint on the silicon wafer by adopting a spraying process, wherein the spraying thickness is 1 mu m, so as to obtain the silicon wafer with the waterproof heat-conducting coating; wherein the area of the silicon wafer is 1cm2
S3, detection:
s3-1: and (3) detecting the waterproof performance: a silicon wafer with a waterproof heat-conducting coating is used for carrying out contact angle test, and the result shows that the contact angle is about 120 degrees; water was dropped on the surface of the silicon wafer having the waterproof heat conductive coating, and it was observed that the shape thereof remained substantially spherical and did not wet the surface of the coating.
S3-2: and (3) detecting the heat conducting property: and (3) carrying out thermal imaging test on the silicon wafer with the waterproof heat-conducting coating on a thermal platform, and detecting the heat-conducting property of the silicon wafer.
Comparative example 1
The comparative example 1 produced a coating, the preparation and performance testing procedures were as follows:
s1, preparing the coating, which specifically comprises the following substeps:
s1-1, preparing materials: the components are prepared according to the following parts by weight: 7 parts of silicon-fluorine resin, 0 part of nano-scale hydrophobic silicon dioxide, 2 parts of few-layer boron nitride and 437.5 parts of ethyl acetoacetate;
s1-2, mixing and stirring: the components are uniformly mixed, poured into a high-speed stirrer, and stirred for 8min at the rotating speed of 1500r/min to obtain the waterproof heat-conducting coating.
S2, spraying: spraying waterproof heat-conducting paint on the silicon wafer by adopting a spraying process, wherein the spraying thickness is 1 mu m, so as to obtain the silicon wafer with the waterproof heat-conducting coating; wherein the area of the silicon wafer is 1cm2
S3, detection:
s3-1: and (3) detecting the waterproof performance: a contact angle test is carried out on the silicon chip with the waterproof heat-conducting coating, and the result shows that the contact angle is less than 120 degrees; when the water drops on the surface of the silicon chip with the waterproof heat-conducting coating, the shape of the silicon chip cannot be kept spherical, the surface of the coating is wetted, and the waterproof performance is poor.
S3-2: and (3) detecting the heat conducting property: and (3) carrying out thermal imaging test on the silicon wafer with the waterproof heat-conducting coating on a thermal platform, and detecting the heat-conducting property of the silicon wafer.
Comparative example 2
The comparative example 2 produces a coating, the preparation and performance testing processes are as follows:
s1, preparing the coating, which specifically comprises the following substeps:
s1-1, preparing materials: the components are prepared according to the following parts by weight: 7 parts of silicon-fluorine resin, 0 part of nano-scale hydrophobic silicon dioxide, 0 part of few-layer boron nitride and 437.5 parts of ethyl acetoacetate;
s1-2, mixing and stirring: the components are uniformly mixed, poured into a high-speed stirrer, and stirred for 8min at the rotating speed of 1500r/min to obtain the waterproof heat-conducting coating.
S2, spraying: spraying waterproof heat-conducting paint on the silicon wafer by adopting a spraying process, wherein the spraying thickness is 1 mu m, so as to obtain the silicon wafer with the waterproof heat-conducting coating; wherein the area of the silicon wafer is 1cm2
S3, detection:
s3-1: and (3) detecting the waterproof performance: the contact angle test is carried out on the silicon chip with the waterproof heat-conducting coating, and the result shows that the contact angle is below 120 degrees, even lower than 100 degrees; when the water drops on the surface of the silicon chip with the waterproof heat-conducting coating, the shape of the silicon chip cannot keep a spherical shape, and the silicon chip wets the surface of the coating and does not have waterproof performance.
S3-2: and (3) detecting the heat conducting property: and (3) carrying out thermal imaging test on the silicon wafer with the waterproof heat-conducting coating on a thermal platform, and detecting the heat-conducting property of the silicon wafer.
Comparative example 3
The waterproof heat-conducting coating prepared in the comparative example 3 is prepared in the following preparation and performance detection processes:
s1, preparing the waterproof heat-conducting paint, which specifically comprises the following substeps:
s1-1, preparing materials: the components are prepared according to the following parts by weight: 7 parts of silicon-fluorine resin, 2.1 parts of nano-scale hydrophobic silicon dioxide, 1 part of few-layer boron nitride and 437.5 parts of ethyl acetoacetate;
s1-2, mixing and stirring: the components are uniformly mixed, poured into a high-speed stirrer, and stirred for 8min at the rotating speed of 1500r/min to obtain the waterproof heat-conducting coating.
S2, spraying: spraying waterproof heat-conducting paint on the silicon wafer by adopting a spraying process, wherein the spraying thickness is 1 mu m, so as to obtain the silicon wafer with the waterproof heat-conducting coating; wherein the area of the silicon wafer is 1cm2
S3, detection:
s3-1: and (3) detecting the waterproof performance: a silicon wafer with a waterproof heat-conducting coating is used for carrying out contact angle test, and the result shows that the contact angle is about 120 degrees; water was dropped on the surface of the silicon wafer having the waterproof heat conductive coating, and it was observed that the shape thereof remained substantially spherical and did not wet the surface of the coating.
S3-2: and (3) detecting the heat conducting property: and (3) carrying out thermal imaging test on the silicon wafer with the waterproof heat-conducting coating on a thermal platform, and detecting the heat-conducting property of the silicon wafer.
Comparative example 4
The waterproof heat-conducting coating prepared in the comparative example 4 is prepared through the following preparation and performance detection processes:
s1, preparing the waterproof heat-conducting paint, which specifically comprises the following substeps:
s1-1, preparing materials: the components are prepared according to the following parts by weight: 7 parts of silicon-fluorine resin, 1.5 parts of nano-scale hydrophobic silicon dioxide, 1.2 parts of few-layer boron nitride and 437.5 parts of ethyl acetoacetate;
s1-2, mixing and stirring: the components are uniformly mixed, poured into a high-speed stirrer, and stirred for 8min at the rotating speed of 1500r/min to obtain the waterproof heat-conducting coating.
S2, spraying: spraying waterproof heat-conducting paint on the silicon wafer by adopting a spraying process, wherein the spraying thickness is 1 mu m, so as to obtain the silicon wafer with the waterproof heat-conducting coating; wherein the area of the silicon wafer is 1cm2
S3, detection:
s3-1: and (3) detecting the waterproof performance: a contact angle test is carried out on the silicon chip with the waterproof heat-conducting coating, and the result shows that the contact angle is less than 120 degrees; when water drops on the surface of the silicon wafer with the waterproof heat-conducting coating, the shape of the water drops cannot be kept spherical, and the water drops partially wet the surface of the coating.
S3-2: and (3) detecting the heat conducting property: and (3) carrying out thermal imaging test on the silicon wafer with the waterproof heat-conducting coating on a thermal platform, and detecting the heat-conducting property of the silicon wafer.
The silicon wafers having the coating layers obtained in examples 1 to 2 and comparative examples 1 to 4 were subjected to contact angle measurement 5 times, respectively, and the average value was calculated. The contact angle test results are shown in the following table:
1 2 3 4 5 average
Example 1 127.29 121.81 126.06 126.44 126.598 126.598
Example 2 120.87 128.03 121.85 120.09 120.67 122.302
Comparative example 1 104.44 101.62 102.37 100.38 99.7 101.702
Comparative example 2 104 99.33 102.52 99.16 100.862 100.862
Comparative example 3 118.87 122.03 120.85 119.09 120.67 120.302
Comparative example 4 106.87 115.03 109.85 110.09 113.67 111.102
The silicon wafers having the coating layers obtained in examples 1 to 2 and comparative examples 1 to 4 were placed on a hot stage, respectively, and their temperature distributions at a suitable time point during the temperature increase were measured. Test results As shown in FIGS. 1 and 2, P1 to P5 in FIG. 1 are the test results of the coated silicon wafer obtained in example 1, the average temperature of the silicon wafer is 46.08 ℃, P6 to P10 in FIG. 1 are the test results of the coated silicon wafer obtained in example 2, the average temperature of the silicon wafer is 46.34 ℃, P11 to P15 in FIG. 1 are the test results of the coated silicon wafer obtained in comparative example 1, the average temperature of the silicon wafer is 45.88 ℃, P1 to P3 in FIG. 2 are the test results of the coated silicon wafer obtained in comparative example 2, the average temperature of the silicon wafer is 43.56 ℃, P4 to P6 in FIG. 2 are the test results of the coated silicon wafer obtained in comparative example 3, the average temperature of the silicon wafer is 44.2 ℃, P7 to P9 in FIG. 2 are the test results of the coated silicon wafer obtained in comparative example 4, and the average temperature of the silicon wafer is 44.37 ℃. As can be seen from the above examples and comparative columns, the coating added with nano-scale hydrophobic silicon dioxide and few layers of boron nitride has the fastest contact angle of more than 120 degrees and the fastest surface temperature rise when being sprayed on a silicon wafer, and has the best waterproof performance and heat-conducting performance. The nano-scale hydrophobic silicon dioxide is used as hydrophobic powder to generate a nano rough structure on the surface of the coating, the silicon fluorine resin is used for modifying the nano rough structure and bonding a few layers of boron nitride, and the few layers of boron nitride are used as a reinforcing phase to play a role in enhancing heat conduction, so that the surface of the coating has good waterproof and heat dissipation properties.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The waterproof heat-conducting coating is characterized by comprising the following components in parts by weight:
6-8 parts of fluorinated resin, 1-3 parts of nanoscale hydrophobic silicon dioxide, 1-3 parts of few-layer boron nitride and 200-500 parts of organic solvent.
2. The waterproof heat-conducting paint as claimed in claim 1, wherein the fluorinated resin is any one of fluorine-modified organosilane, fluorinated epoxy resin, organic silicon polymer resin and silicon fluorine resin.
3. The waterproof heat-conducting paint as claimed in claim 1, wherein the organic solvent includes one or more of ethyl acetoacetate, ethyl acetate and ethanol.
4. A preparation method of the waterproof heat-conducting coating is characterized by comprising the following steps:
s11, preparing the following components in parts by weight: 6-8 parts of fluorinated resin, 1-3 parts of nanoscale hydrophobic silicon dioxide, 1-3 parts of few-layer boron nitride and 200-500 parts of organic solvent;
s12, stirring and mixing the components prepared in the step S11 at a high speed to obtain the waterproof heat-conducting coating.
5. The preparation method of the waterproof heat-conducting coating as claimed in claim 4, wherein the stirring speed of the high-speed stirring in the step S12 is 1300-1700 rpm, and the stirring time is 5-10 min;
the few-layer boron nitride is prepared by the following steps:
mixing single-layer boron nitride with sodium hypochlorite to form mixed slurry, carrying out ball milling on the mixed slurry, and then centrifuging to obtain a lower-layer product;
sequentially cleaning, filtering and drying the lower-layer product to obtain solid particles;
dispersing the solid particles in isopropanol for ultrasonic treatment, and centrifuging to obtain an upper-layer mixed solution;
and filtering and drying the upper layer mixed solution to obtain the few-layer boron nitride.
6. The preparation method of the waterproof heat-conducting coating as claimed in claim 4, wherein when the single-layer boron nitride and the sodium hypochlorite are mixed to form the mixed slurry, the mass ratio of the single-layer boron nitride to the sodium hypochlorite is 1: 50;
when the mixed slurry is subjected to ball milling, the ball milling rotation speed is 150rpm, and the ball milling time is 16 h;
when the lower-layer product is obtained by the centrifugation, the centrifugation rotating speed is 5000rpm, and the centrifugation time is 10 min.
7. The preparation method of the waterproof heat-conducting coating according to claim 4, wherein the lower layer product is sequentially washed, filtered and dried to obtain solid particles, and the preparation method specifically comprises the following steps:
sequentially cleaning the lower-layer product by using three solutions of hydrochloric acid, water and ethanol to obtain a neutral mixed solution;
carrying out suction filtration on the neutral mixed solution by using a filter membrane with the specification of 1.5-2.5 microns to obtain a solid product;
drying the solid product to obtain solid particles.
8. The preparation method of the waterproof heat-conducting coating according to claim 4, wherein when the solid particles are dispersed in isopropanol and subjected to ultrasound, the ratio of the solid particles to the isopropanol is 0.5mg/mL, and the ultrasound time is 0.5 h;
when the upper-layer mixed solution is obtained through centrifugation, the centrifugation rotating speed is 3000rpm, and the centrifugation time is 30 min;
and when the upper-layer mixed solution is filtered and dried, the specification of the filtering membrane is 1.5-2.5 mu m.
9. A preparation method of a waterproof heat-conducting coating is characterized by comprising the following steps: the waterproof thermal conductive coating material according to any one of claims 1 to 3 or the waterproof thermal conductive coating material obtained by the preparation method according to any one of claims 4 to 8 is sprayed on an electronic component by a spray coating process to form a waterproof thermal conductive coating layer.
10. The preparation method of the waterproof heat-conducting coating according to claim 9, wherein the thickness of the waterproof heat-conducting coating is 1-2 μm;
the waterproof heat-conducting coating is sprayed on the electronic component through a spraying process, and then the method further comprises the following steps:
and baking the electronic part sprayed with the waterproof heat-conducting coating for 1-3 hours at 50-70 ℃.
CN202010616288.0A 2020-06-30 2020-06-30 Waterproof heat-conducting coating and preparation method thereof Pending CN111647354A (en)

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