CN115851026B - High-thermal-conductivity insulated electrophoretic paint and preparation method thereof - Google Patents
High-thermal-conductivity insulated electrophoretic paint and preparation method thereof Download PDFInfo
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Abstract
The invention discloses high-heat-conductivity insulated electrophoretic paint and a preparation method thereof. Firstly, adding graphene nano sheets and a dispersing agent into a solvent, and stirring to obtain graphene dispersion liquid; adding hexagonal boron nitride and a dispersing agent into a solvent, stirring to obtain hexagonal boron nitride dispersion liquid, centrifuging, taking supernatant, adding a silane coupling agent hydrolysate, and stirring to obtain a modified hexagonal boron nitride dispersion liquid; then mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid into an additive according to the volume ratio of 1:1-3; finally, the additive is added into the electrophoretic paint to obtain the high-heat-conductivity insulating electrophoretic paint. The electrophoretic paint is used as a bath solution to coat the metal surface, and a magnetic field is applied to the bath solution during coating. The method adopts the combined dispersion liquid of the few layers of hexagonal boron nitride and the graphene nano-sheets to enhance the heat conduction capability of the electrophoretic paint, and adopts the silane coupling agent to carry out chemical connection on the functional additive, so that the metal coating has good insulativity and heat conduction performance.
Description
Technical Field
The invention belongs to the technical field of metal surface coatings, and particularly relates to high-heat-conductivity insulated electrophoretic paint and a preparation method thereof.
Background
Heat dissipation is a key technology in the use of trolley batteries, electronic components, satellites, and the like. Graphene is the material with the highest heat conductivity coefficient up to now, which is higher than that of single-wall carbon nanotubes (3500W/m.K) and multi-wall carbon nanotubes (3000W/m.K), and the heat conductivity coefficient of pure defect-free single-layer graphene is as high as 5300W/mK, which means that the material is 1m thick, the temperature difference between the two side surfaces is 1K, and the heat transferred through 1 square meter area can reach 5300W in 1 second. The thermal conductivity of the graphene thermal conductive film and the graphene coating can also reach 600W/m.K. Meanwhile, graphene also has excellent conductivity.
At present, electric automobiles gradually become development trend of modern and future automobile industry, and the battery can still reliably and permanently work under the use environment temperature, and the heat dissipation capability becomes an important limiting factor affecting the service life of the battery. At present, the cooling technology of the electric automobile mainly adopts air cooling and water cooling. Air cooling is introduced, the volume is increased, noise is generated, and the stability of the operation of the fan is increased by an additional unstable factor; the prior technology of intensive liquid cooling with high requirements is not mature, and the prior air cooling and liquid cooling technology has complex system, heavy weight, great maintenance difficulty and possibility of liquid leakage. Meanwhile, other ways of improving heat dissipation have a series of problems: increasing the heat dissipation area inevitably leads to volume increase and weight increase, leads to energy consumption increase and operation stability reduction, and leads to carbon dioxide emission increase; material replacement, such as replacement of aluminum by copper, has limited lifting, obviously increased weight and obviously increased cost; the heat pipe is introduced, so that concentrated heat can be quickly conducted away basically, but if heat dissipation is not timely carried out, the cold end and the hot end of the heat pipe reach heat balance, and the heat pipe is invalid.
The satellite flying in space has two main sources of heat, one is the heat generated by solar radiation, the other is the heat generated by the operation of parts of the satellite, the two heat are accumulated together in the satellite, if the heat is not dissipated for a long time, the satellite is broken down due to light weight, and the satellite is directly burnt due to heavy weight. The electronic equipment on the aerospace craft has the characteristics of small volume, light weight and low power consumption, and for small and medium-sized civil and commercial aerospace satellites, the design concept of compactness and miniaturization of the electronic equipment causes that a plurality of electronic elements are integrated in smaller and smaller areas, so that the heat flux density is increased sharply, and in addition, the special environmental conditions are adopted, so that the heat dissipation and heat preservation of the electronic device are more difficult. The satellite has relatively low thermal control technology level, and generally has the problems of high cost, long development period and the like.
Disclosure of Invention
The invention aims to provide a preparation method of high-thermal-conductivity insulated electrophoretic paint.
The method of the invention is as follows:
step (1) preparing graphene dispersion liquid:
adding graphene nano-sheets GNP and a dispersing agent into a solvent, and uniformly stirring by using high-shear equipment at normal temperature to obtain graphene dispersion liquid. The stirring time of the high shearing equipment is 2-3 hours, and the rotating speed is 5000-8000 rpm.
The transverse dimension of the graphene nano-sheet GNP is 0.1-1.0 mu m, and the number of layers is 11-200. 2.0-20.0 g graphene nanoplatelets GNP, preferably 5.0-10.0 g, are added per liter of solvent. 0.02-0.5 g of dispersant, preferably 0.05-0.2 g, is added for each gram of graphene nano-sheet GNP.
After stirring by high shearing equipment, the graphene nano sheets GNP are further peeled off, the number of layers of the graphene nano sheets GNP is reduced, part of the graphene nano sheets GNP are converted into fewer layers of graphene FLG with the number of layers being less than or equal to 10, the FLG/GNP are uniformly dispersed, and agglomeration is avoided under the action of space electrostatic repulsion. The smaller the number of graphene layers, the higher the thermal conductivity.
Step (2) preparing modified hexagonal boron nitride dispersion liquid:
adding hexagonal boron nitride h-BN and a dispersing agent into a solvent, and uniformly stirring by using high-shear equipment at normal temperature to obtain hexagonal boron nitride dispersion liquid. Stirring time is 4-5 hours, and the rotating speed is 5000-8000 rpm.
The lateral dimension of the hexagonal boron nitride h-BN is 0.1-1.0 mu m, and the number of layers is 11-100. 2.0 to 20.0g of hexagonal boron nitride h-BN, preferably 5.0 to 10.0g, is added per liter of solvent. The dispersant is added in the amount of 0.02-0.5 g, preferably 0.05-0.2 g, for each gram of hexagonal boron nitride h-BN.
After stirring by high shearing equipment, the hexagonal boron nitride h-BN is further stripped, the number of layers of the hexagonal boron nitride h-BN is reduced, part of the hexagonal boron nitride h-BN is converted into hexagonal boron nitride h-BN with the number of layers being less than or equal to 10, and the hexagonal boron nitride h-BN with multiple layers is uniformly dispersed and does not agglomerate under the action of space electrostatic repulsion. The smaller the number of layers of hexagonal boron nitride h-BN, the higher the thermal conductivity.
Centrifuging the hexagonal boron nitride dispersion liquid for 10-60 minutes at 4000-6000 rpm, taking supernatant, adding the silane coupling agent hydrolysate, and stirring for 2-3 hours at normal temperature to connect the hexagonal boron nitride h-BN with the silane coupling agent to obtain the modified hexagonal boron nitride dispersion liquid.
The silane coupling agent hydrolysate is a silane coupling agent aqueous solution with the mass fraction of 2-8%, and the silane coupling agent is amino or epoxy silane coupling agent, preferably one of N- (beta-aminoethyl) -gamma-aminopropyl triethoxy silane, gamma-aminopropyl methyl diethoxy silane, gamma-aminopropyl trimethoxy silane, aminopropyl triethoxy silane and gamma- (3, 2-epoxypropoxy) propyl trimethoxy silane. Adding 0.4-4.0 g of silane coupling agent hydrolysate into each liter of supernatant.
The solvent adopted in the step (1) and the step (2) is the same, and is one of water, ethylene glycol butyl ether BCS, methyl isobutyl ketone MIBK, ethylene glycol tertiary butyl ether ETB, isopropyl alcohol IPA and N-methyl pyrrolidone NMP.
The dispersant adopted in the step (1) and the step (2) is the same, and is a polymer surfactant, preferably one of BYK-3560, BYK-4509 and BYK-4510.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to the volume ratio of 1:1-3 to form the additive.
And (4) uniformly mixing the additive with the electrophoretic paint to obtain the high-heat-conductivity insulating electrophoretic paint. 1-100 g of additive is added into each kilogram of electrophoretic paint; preferably 5 to 50 g.
The invention also aims to provide the high-thermal conductivity insulated electrophoretic paint prepared by the method, which has a pH value of 5.4-6.2 and an electrical conductivity of 1000-2000 mu S/cm. The electrophoretic paint can be used for insulating coatings for heat dissipation of electric automobiles (battery boxes), satellites, space stations, electronic elements and the like.
And (3) using the prepared electrophoretic paint as a bath solution to coat the metal surface. During coating, a planar metal plate to be coated is vertically placed in a bath solution, a thick magnet is placed outside one side of an electrophoresis tank workpiece, a magnetic field is applied to the bath solution, so that the graphene plane in the electrophoresis coating of the metal plate is perpendicular to the surface plane of the workpiece, the heat dissipation of the metal surface coating is improved, and the strength of the magnetic field is 0.1-1.0 Tesla. Electrophoretic coating process parameters: the electrophoresis voltage is direct current voltage or pulse voltage of 60-160V, the electrophoresis time is 60-240 s, and the temperature of the bath solution is 25-32 ℃.
The method adopts the combined dispersion liquid of the few-layer hexagonal boron nitride h-BN and the graphene nano-sheet GNP which are stable under the steric hindrance repulsive force to enhance the heat conduction capability of the electrophoretic paint, and uses the silane coupling agent to carry out chemical connection on the functional additive. The h-BN has good insulativity and heat conduction performance at room temperature, the GNP has good electric conductivity and heat conduction, the h-BN and the FLG can achieve good insulation effect after being connected in a chemical mode, the requirement of coating insulation in certain applications is met, meanwhile, an externally applied magnetic field can promote the oriented arrangement of graphene perpendicular to a substrate plane (the graphene heat dissipation effect is best in the arrangement mode), compared with a pure epoxy resin coating, the preparation method of the GNP/h-BN composite coating adopted by the method can improve the heat conduction at room temperature by more than 100 times (from 0.2W/(m.K) to 30W/(m.K)), and the surface volume resistivity of the coating is more than 1010 Ω.m.
Detailed Description
The invention is further illustrated below with reference to examples. The lateral dimension of the graphene nanoplatelets GNP used in the following examples is 0.1-1.0 μm, and the number of layers is 11-200; the lateral dimension of the hexagonal boron nitride h-BN is 0.1-1.0 mu m, and the number of layers is 11-100.
Example 1.
And (1) adding 2.0g of graphene nano-sheets GNP and 1.0g of dispersant BYK-3560 into 1 liter of water, and stirring for 3 hours at normal temperature by using high shear equipment, wherein the rotating speed is 5000 r/h, so as to obtain graphene dispersion liquid.
Adding 6.0g of hexagonal boron nitride h-BN and 1.8g of dispersant BYK-3560 into 1 liter of water, stirring for 4.5 hours at normal temperature by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at the rotating speed of 6000 rpm; centrifuging the hexagonal boron nitride dispersion liquid for 10 minutes at the rotating speed of 6000 rpm, and taking supernatant; and then adding an N- (beta-aminoethyl) -gamma-aminopropyl triethoxysilane aqueous solution with the mass fraction of 8% according to the proportion of 0.4g per liter of supernatant, and stirring for 150 minutes at normal temperature to obtain the modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 1:2 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 1:50 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoretic paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.1 Tesla to the bath solution to enable the graphene plane in the metal plate electrophoresis coating to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 160V DC voltage, the electrophoresis time is 60s, the bath solution temperature is 27 ℃, and the film thickness of the electrophoresis paint composite coating is 22 mu m.
Example 2.
And (1) adding 5.0g of graphene nanoplatelets GNP and 2.0g of dispersant BYK-4509 into 1 liter of ethylene glycol butyl ether solvent, stirring at normal temperature for 170 minutes by using high shearing equipment, and obtaining graphene dispersion liquid at the rotating speed of 5500 r/h.
Step (2) adding 8.0g of hexagonal boron nitride h-BN and 1.6g of dispersant BYK-4509 into 1 liter of ethylene glycol butyl ether solvent, stirring for 260 minutes at normal temperature by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at a rotating speed of 7000 r/h; centrifuging the hexagonal boron nitride dispersion liquid for 15 minutes at the rotating speed of 5800 r/h, and taking supernatant; then adding a gamma-aminopropyl methyl diethoxy silane aqueous solution with the mass fraction of 7% according to the proportion of 1.0g per liter of supernatant, and stirring for 3 hours at normal temperature to obtain the modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 2:3 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 3:100 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoresis paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.2 Tesla to the bath solution to enable the graphene plane in the electrophoresis coating of the metal plate to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 140V pulse voltage, the electrophoresis time is 80s, the bath solution temperature is 30 ℃, and the film thickness of the electrophoresis paint composite coating is 23 mu m.
Example 3.
And (1) adding 6.0g of graphene nanoplatelets GNP and 1.8g of dispersant BYK-4510 into 1 liter of methyl isobutyl ketone solvent, stirring at normal temperature for 160 minutes by using high shear equipment, and obtaining graphene dispersion liquid at the rotating speed of 6000 rpm.
Adding 2.0g of hexagonal boron nitride h-BN and 1.0g of dispersant BYK-4510 into 1 liter of methyl isobutyl ketone solvent, stirring at normal temperature for 5 hours by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at a rotation speed of 5000 r/h; centrifuging the hexagonal boron nitride dispersion liquid for 20 minutes at the rotating speed of 5500 r/h, and taking supernatant; and then adding a gamma-aminopropyl trimethoxysilane aqueous solution with the mass fraction of 6% according to the proportion of 1.5g per liter of supernatant, and stirring for 2 hours at normal temperature to obtain the modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 1:1 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 1:1000 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoretic paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.3 Tesla to the bath solution to enable the graphene plane in the metal plate electrophoresis coating to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 120V DC voltage, the electrophoresis time is 100s, the bath solution temperature is 25 ℃, and the film thickness of the electrophoresis paint composite coating is 24.5 mu m.
Example 4.
And (1) adding 8.0g of graphene nano-sheets GNP and 1.6g of dispersant BYK-3560 into 1 liter of ethylene glycol tertiary butyl ether solvent, and stirring for 2.5 hours at normal temperature by using high shear equipment at the rotating speed of 6500 r/h to obtain graphene dispersion liquid.
Adding 5.0g of hexagonal boron nitride h-BN and 2.0g of dispersant BYK-3560 into 1 liter of ethylene glycol tertiary butyl ether solvent, stirring at normal temperature for 250 minutes by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at the rotating speed of 7500 r/h; centrifuging the hexagonal boron nitride dispersion liquid for 30 minutes at the rotation speed of 5000 rpm, and taking supernatant; and adding 2.0g of aminopropyl triethoxysilane aqueous solution with the mass fraction of 5% into each liter of supernatant, and stirring at normal temperature for 160 minutes to obtain modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 1:3 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 1:200 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoresis paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.4 Tesla to the bath solution to enable the graphene plane in the electrophoresis coating of the metal plate to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 100V pulse voltage, the electrophoresis time is 120s, the bath solution temperature is 28 ℃, and the film thickness of the electrophoresis paint composite coating is 25 mu m.
Example 5.
And (1) adding 10.0g of graphene nanoplatelets GNP and 0.8g of dispersant BYK-4509 into 1 liter of isopropanol solvent, stirring for 140 minutes at normal temperature by using high shear equipment, and obtaining graphene dispersion liquid at a rotating speed of 7000 r/h.
Adding 16.0g of hexagonal boron nitride h-BN and 0.8g of dispersant BYK-4509 into 1 liter of isopropanol solvent, stirring for 290 minutes at normal temperature by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at the rotating speed of 5500 r/h; centrifuging the hexagonal boron nitride dispersion liquid for 40 minutes at the rotation speed of 5000 rpm, and taking supernatant; and adding 2.5g of gamma- (3, 2-glycidoxy) propyl trimethoxy silane aqueous solution with the mass fraction of 4% into each liter of supernatant, and stirring for 140 minutes at normal temperature to obtain modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 2:5 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 1:20 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoretic paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.5 Tesla to the bath solution to enable the graphene plane in the metal plate electrophoresis coating to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 90V DC voltage, the electrophoresis time is 140s, the bath solution temperature is 32 ℃, and the film thickness of the electrophoresis paint composite coating is 23 mu m.
Example 6.
And (1) adding 12.0g of graphene nano-sheets GNP and 1.2g of dispersant BYK-4510 into 1 liter of N-methylpyrrolidone solvent, stirring at normal temperature for 250 minutes by using high shear equipment, and obtaining graphene dispersion liquid at the rotating speed of 7500 r/h.
Step (2) adding 20.0g of hexagonal boron nitride h-BN and 0.4g of dispersant BYK-4510 into 1 liter of N-methylpyrrolidone solvent, stirring for 280 minutes at normal temperature by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at the rotating speed of 6000 rpm; centrifuging the hexagonal boron nitride dispersion liquid for 45 minutes at the rotation speed of 5000 rpm, and taking supernatant; then adding an N- (beta-aminoethyl) -gamma-aminopropyl triethoxysilane aqueous solution with the mass fraction of 4% according to the proportion of 3.0g per liter of supernatant, and stirring for 2.5 hours at normal temperature to obtain the modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 1:2 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 2:25 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoretic paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.6 Tesla to the bath solution to enable the graphene plane in the metal plate electrophoresis coating to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 80V pulse voltage, the electrophoresis time is 160min, the bath solution temperature is 25 ℃, and the film thickness of the electrophoresis paint composite coating is 22 mu m.
Example 7.
And (1) adding 16.0g of graphene nano-sheets GNP and 0.8g of dispersant BYK-3560 into 1 liter of water, and stirring for 2 hours at normal temperature by using high shear equipment, wherein the rotating speed is 8000 revolutions per hour, so as to obtain graphene dispersion liquid.
Adding 12.0g of hexagonal boron nitride h-BN and 1.2g of dispersant BYK-3560 into 1 liter of water, stirring for 4 hours at normal temperature by using high shearing equipment, and obtaining hexagonal boron nitride dispersion liquid at the rotating speed of 8000 revolutions per hour; centrifuging the hexagonal boron nitride dispersion liquid for 50 minutes at the rotating speed of 4500 rpm, and taking supernatant; then adding 3.5g of gamma-aminopropyl methyl diethoxy silane aqueous solution with the mass fraction of 3% into each liter of supernatant, and stirring for 3 hours at normal temperature to obtain modified hexagonal boron nitride dispersion.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 2:3 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 1:100 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoretic paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 0.8 Tesla to the bath solution to enable the graphene plane in the metal plate electrophoresis coating to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 70V DC voltage, the electrophoresis time is 180s, the bath solution temperature is 30 ℃, and the film thickness of the electrophoresis paint composite coating is 21 mu m.
Example 8.
And (1) adding 20.0g of graphene nanoplatelets GNP and 0.4g of dispersant BYK-4509 into 1 liter of isopropanol solvent, stirring for 120 minutes at normal temperature by using high shear equipment, and obtaining graphene dispersion liquid at the rotating speed of 6000 rpm.
Step (2) adding 10.0g of hexagonal boron nitride h-BN and 0.8g of dispersant BYK-4509 into 1 liter of isopropanol solvent, stirring for 4.5 hours at normal temperature by using high shear equipment, and obtaining hexagonal boron nitride dispersion liquid at the rotating speed of 6500 r/h; centrifuging the hexagonal boron nitride dispersion liquid for 60 minutes at the rotating speed of 4000 rpm, and taking supernatant; and adding an aminopropyl triethoxysilane aqueous solution with the mass fraction of 2% according to the proportion of 4.0g per liter of supernatant, and stirring for 2 hours at normal temperature to obtain the modified hexagonal boron nitride dispersion liquid.
And (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid according to a volume ratio of 2:5 to form the additive.
And (4) uniformly mixing the additive and the electrophoretic paint according to the mass ratio of 1:10 to obtain the high-heat-conductivity insulating electrophoretic paint.
And taking the prepared high-heat-conductivity insulating electrophoretic paint as a bath solution, vertically placing a planar metal plate to be coated in the bath solution, placing a thick magnet outside one side of an electrophoresis tank workpiece, and applying a magnetic field with the strength of 1.0 Tesla to the bath solution to enable the graphene plane in the metal plate electrophoresis coating to be perpendicular to the surface plane of the workpiece. Electrophoretic coating process parameters: the electrophoresis voltage is 60V pulse voltage, the electrophoresis time is 240s, the bath solution temperature is 26 ℃, and the film thickness of the electrophoresis paint composite coating is 20 mu m.
Comparative example.
The procedure was the same as in example 1, except that the mixed additives of graphene and h-BN were not added to the bath solution.
The electrophoretic paints prepared in examples 1 to 8 and comparative examples were tested for resistivity and thermal conductivity, test methods: the surface resistivity test of the electrophoretic paint is detected according to the HG/T3331-2012 standard; the thermal conductivity test is carried out according to the GB/T22588-2008 standard. The test results are shown in the following table:
as can be seen from the table, the invention combines the graphene and the h-BN by adding the silane coupling agent, and well disperses the graphene and the h-BN mixed additive in the electrophoretic paint. The electrophoretic paint prepared by the invention has the advantages of insulation, obviously improved heat conductivity coefficient and higher stability.
Claims (9)
1. A preparation method of high-heat-conductivity insulated electrophoretic paint is characterized by comprising the following steps of:
step (1) preparing graphene dispersion liquid:
adding graphene nano-sheets GNP and a dispersing agent into a solvent, and stirring by using high-shear equipment at normal temperature to obtain graphene dispersion; 2.0-20.0 g of graphene nano-sheets GNP are added into each liter of solvent, and 0.02-0.5 g of dispersing agent is correspondingly added into each gram of graphene nano-sheets GNP; the transverse dimension of the graphene nano sheet GNP is 0.1-1.0 mu m, and the number of layers is 11-200;
step (2) preparing modified hexagonal boron nitride dispersion liquid:
adding hexagonal boron nitride h-BN and a dispersing agent into a solvent, and stirring by using high shear equipment at normal temperature to obtain hexagonal boron nitride dispersion; adding 2.0-20.0 g of hexagonal boron nitride h-BN into each liter of solvent, and correspondingly adding 0.02-0.5 g of dispersing agent into each gram of hexagonal boron nitride h-BN;
centrifuging the hexagonal boron nitride dispersion liquid, taking supernatant, adding a silane coupling agent hydrolysate, and stirring for 2-3 hours at normal temperature to obtain a modified hexagonal boron nitride dispersion liquid; the silane coupling agent hydrolysate is a silane coupling agent aqueous solution with the mass fraction of 2-8%, the silane coupling agent is amino or epoxy silane coupling agent, and 0.4-4.0 g of the silane coupling agent hydrolysate is added into each liter of supernatant;
the dispersant adopted in the step (1) and the step (2) is the same and is a macromolecular surfactant;
the solvent adopted in the step (1) and the step (2) is the same, and is one of water, ethylene glycol butyl ether BCS, methyl isobutyl ketone MIBK, ethylene glycol tertiary butyl ether ETB, isopropyl alcohol IPA and N-methyl pyrrolidone NMP;
step (3) mixing the graphene dispersion liquid and the modified hexagonal boron nitride dispersion liquid into an additive according to the volume ratio of 1:1-3;
step (4) uniformly mixing the additive and the electrophoretic paint to obtain the high-heat-conductivity insulating electrophoretic paint; 1-100 g of additive is added into each kilogram of electrophoretic paint.
2. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: the stirring time of the high shearing equipment in the step (1) is 2-3 hours, and the rotating speed is 5000-8000 rpm.
3. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: in the step (1), 5.0-10.0 g of graphene nano-sheets GNP are added per liter of solvent, and 0.05-0.2 g of dispersing agent is correspondingly added per gram of graphene nano-sheets GNP.
4. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: the stirring time of the high shearing equipment in the step (2) is 4-5 hours, and the rotating speed is 5000-8000 rpm.
5. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: in the step (2), 5.0-10.0 g of hexagonal boron nitride h-BN is added per liter of solvent, and 0.05-0.2 g of dispersing agent is correspondingly added per gram of hexagonal boron nitride h-BN.
6. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the hexagonal boron nitride dispersion liquid is centrifuged for 10 to 60 minutes, and the rotating speed is 4000 to 6000 revolutions per hour.
7. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: the silane coupling agent is one of N- (beta-aminoethyl) -gamma-aminopropyl triethoxysilane, gamma-aminopropyl methyl diethoxysilane, gamma-aminopropyl trimethoxysilane, aminopropyl triethoxysilane and gamma- (3, 2-epoxypropoxy) propyl trimethoxysilane.
8. The method for preparing the high-thermal-conductivity insulating electrophoretic paint as claimed in claim 1, wherein the method comprises the following steps: in the step (4), 5-50 g of additive is added into each kilogram of electrophoretic paint.
9. The high thermal conductivity insulated electrophoretic paint prepared by the method of any one of claims 1-8, wherein the pH value is 5.4-6.2, and the electrical conductivity is 1000-2000 mu S/cm.
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