CN114479614A - Water-based graphene composite heat dissipation coating and preparation method thereof - Google Patents
Water-based graphene composite heat dissipation coating and preparation method thereof Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Paints Or Removers (AREA)
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Abstract
The invention relates to a water-based graphene composite heat dissipation coating and a preparation method thereof. The water-based graphene composite heat dissipation coating comprises a component A and a component B; the component A comprises reduced graphene oxide slurry, water-based epoxy resin, heat-conducting filler, an auxiliary agent and water; wherein the reduced graphene oxide slurry is prepared by thermally reducing an aqueous solution of graphene oxide; the Mohs hardness of the heat-conducting filler is not less than 7; the component B comprises an epoxy curing agent and water. The water-based graphene composite heat dissipation coating has a good heat dissipation effect.
Description
Technical Field
The invention relates to the technical field of heat dissipation coatings, in particular to a water-based graphene composite heat dissipation coating and a preparation method thereof.
Background
With the development of electronic circuits and communication technologies, electronic devices and high-performance chips have been increasingly miniaturized, light-weighted, and efficient. The size of the device is gradually reduced, and the heat dissipation problem is also gradually severe. The high temperature generated by poor heat dissipation can not only lead the equipment to be unstable in operation and shorten the service life, but also lead some parts to be burnt. Therefore, the heat dissipation problem is a bottleneck limiting the development of lightweight high performance devices. The current market mainly solves the electronic element heat dissipation problem with fin heat dissipation, but the fin radiator is limited by volume and mass, and the heat dissipation efficiency is limited, and the heat dissipation requirement of the high-power electronic element is difficult to meet.
Aiming at the rigor of the heat dissipation problem, the heat dissipation coating can be applied to the electronic field to solve the heat dissipation problem. Due to the fact that graphene has extremely high heat conductivity coefficient and strong radiance (the heat conductivity coefficient can reach 5300W/m.K, and the radiance coefficient is more than 0.9), after the graphene heat dissipation coating prepared by taking graphene as a raw material is coated on the surface of a base material, the heat radiation coefficient of the surface of the base material (more than 0.9) can be greatly improved, and the heat exchange efficiency of the surface of an object is greatly improved. Simultaneously, the heat on the surface of the substrate is rapidly taken away by the graphene heat dissipation coating in an infrared radiation mode, so that the heat exchange effect is improved, and the surface and internal temperature of an object is reduced.
However, graphene has a high aspect ratio, high van der waals force existing between sheets, and weak pi-pi interaction between aromatic rings, so that it is easily agglomerated and hardly uniformly dispersed in water and organic solvents by means of chemical bonding. It hardly forms stable bonding with a polymer, which results in weak interfacial bonding force between a resin and graphene in a coating material, thereby making compatibility thereof poor, making graphene easily aggregated and poor dispersibility in water, and affecting its function and performance in a coating layer to the maximum.
Disclosure of Invention
Based on the above, the invention provides a water-based graphene composite heat dissipation coating and a preparation method thereof. The problem of poor heat dispersion of the water-based graphene coating is solved.
The first aspect of the invention provides a water-based graphene composite heat dissipation coating, which has the following technical scheme:
a water-based graphene composite heat dissipation coating comprises a component A and a component B;
the component A comprises reduced graphene oxide slurry, water-based epoxy resin, heat-conducting filler, an auxiliary agent and water;
wherein the reduced graphene oxide slurry is prepared by thermally reducing an aqueous solution of graphene oxide;
the Mohs hardness of the heat-conducting filler is not less than 7;
the component B comprises an epoxy curing agent and water.
In some embodiments, the method for preparing reduced graphene oxide comprises the following steps:
and carrying out reduction reaction on the aqueous solution of the graphene oxide for 1-4 h at the temperature of 200-500 ℃ and under the pressure of 123-309 KPa.
In some of these embodiments, the method of preparing reduced graphene oxide does not include the step of adding a reducing agent.
In some embodiments, the mass concentration of the aqueous solution of graphene oxide is 0.5% to 10%, and the amount ratio of carbon-oxygen substances in the graphene oxide is (1.2-2.0): 1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
In some of these embodiments, the thermally conductive filler is selected from alumina and/or silicon carbide.
In some of these embodiments, the alumina has a particle size of 2 μm to 20 μm.
In some of these embodiments, the silicon carbide has a particle size of 2 μm to 20 μm.
In some of these embodiments, the thermally conductive filler is a combination of aluminum oxide and silicon carbide, and the mass ratio of aluminum oxide to silicon carbide is n: (10-n), wherein n is any value excluding 10 in the range of 5-10.
In some of these embodiments, the waterborne epoxy resin has a solids content of 40% to 70%.
In some of these embodiments, the adjuvant is selected from at least one of a dispersant, a wetting agent, an aqueous rheology adjuvant, a defoamer, and a thickener.
In some of these embodiments, the dispersant is selected from at least one of carboxylate dispersants, aliphatic amide dispersants, and ester dispersants.
In some of these embodiments, the wetting agent is selected from at least one of sodium dodecylbenzene sulfonate, fluorinated polyacrylate, polyoxyethylene octylphenol ether, and polyoxyethylene alkyl acid ether.
In some of these embodiments, the aqueous rheology aid is selected from at least one of polyacrylic acid and polyether modified polysiloxane.
In some of these embodiments, the defoamer is selected from at least one of mineral oil and silicone.
In some of these embodiments, the thickener is selected from at least one of an acrylic-type thickener, a polyurethane-type thickener, and bentonite.
In some of these embodiments, the epoxy curing agent is selected from at least one of methylenedicyclohexylamine and isophorone diamine.
In some embodiments, the component a comprises the following preparation raw materials in parts by weight:
10-100 parts of reduced graphene oxide slurry, 200-500 parts of water-based epoxy resin, 200-450 parts of heat-conducting filler, 18-120 parts of assistant and 50-200 parts of water.
The component B comprises the following preparation raw materials in parts by weight:
50-200 parts of epoxy curing agent and 800-950 parts of water.
In some embodiments, the auxiliary comprises the following components in parts by weight:
5-20 parts of dispersing agent, 5-20 parts of wetting agent, 2-40 parts of aqueous rheological additive, 1-10 parts of defoaming agent and 5-30 parts of thickening agent.
The second aspect of the invention provides a preparation method of a water-based graphene composite heat dissipation coating, which adopts the following technical scheme:
a preparation method of a water-based graphene composite heat dissipation coating comprises the following steps:
mixing reduced graphene oxide slurry, an auxiliary agent and water, adding a heat-conducting filler for continuous mixing, adding a water-based epoxy resin for continuous mixing, and preparing a component A;
mixing an epoxy curing agent and water to prepare a component B;
and (2) mixing the component A and the component B according to the mass ratio of (8-15): 1, mixing and curing.
In some embodiments, the curing temperature is 80-150 ℃, and the curing time is 30 min-2 h.
In some embodiments, the rotation speed of the mixed reduced graphene oxide slurry, the auxiliary agent and the water is 400r/min to 1000r/min, and the time is 5min to 20min.
In some embodiments, the rotating speed of adding the heat-conducting filler for continuous mixing is 1500 r/min-2500 r/min, and the time is 20 min-60 min.
In some embodiments, the rotation speed of adding the water-based epoxy resin for continuous mixing is 500 r/min-1000 r/min, and the time is 10 min-30 min.
In some embodiments, the epoxy curing agent and the water are mixed at a rotation speed of 200r/min to 800r/min for 5min to 20min.
The inventor of the present invention finds, by studying factors affecting the heat dissipation performance of the graphene heat dissipation coating, that the heat dissipation performance of the graphene heat dissipation coating is not only related to the dispersibility of graphene in a coating and the compatibility of graphene and a resin, but also the hardness of a heat conductive filler in the coating affects the heat dissipation effect of the graphene heat dissipation coating. Thereby forming the technical scheme of the invention. According to the invention, the heat-conducting filler with proper hardness is selected, and the reduced graphene oxide which has no adverse effect when matched with the heat-conducting filler and can be well dispersed in the coating and well compatible with the epoxy resin is selected, and the component A of the water-based graphene composite heat-dissipating coating is formed together with the water-based epoxy resin and water. The epoxy curing agent and water are used as the component B of the water-based graphene composite heat dissipation coating, and compared with the traditional scheme, the water-based graphene composite heat dissipation coating has a good heat dissipation effect.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Term(s) for
Unless otherwise stated or contradicted, terms or phrases used herein have the following meanings:
as used herein, the term "and/or", "and/or" includes any one of two or more of the associated listed items, as well as any and all combinations of the associated listed items, including any two of the associated listed items, any more of the associated listed items, or all combinations of the associated listed items.
In the present invention, "at least one" means any one, any two or more of the listed items.
In the present invention, "optionally", "optional" and "optional" refer to the presence or absence, i.e., to any one of two juxtapositions selected from "present" and "absent". If multiple optional parts appear in one technical scheme, if no special description exists, and no contradiction or mutual constraint relation exists, each optional part is independent.
In the present invention, "preferred" is only used to describe better embodiments or examples, and it should be understood that the scope of the present invention is not limited by these examples.
In the present invention, the technical features described in the open type include a closed technical solution composed of the listed features, and also include an open technical solution including the listed features.
In the present invention, the numerical range is defined to include both end points of the numerical range unless otherwise specified.
In the present invention, the percentage content refers to both mass percentage for solid-liquid mixing and solid-solid phase mixing and volume percentage for liquid-liquid phase mixing, unless otherwise specified.
In the present invention, the percentage concentrations are referred to as final concentrations unless otherwise specified. The final concentration refers to the ratio of the additive component in the system to which the component is added.
In the present invention, the temperature parameter is not particularly limited, and the treatment is allowed to be performed at a constant temperature or within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
The inventor of the present invention finds, by studying factors affecting the heat dissipation performance of the graphene heat dissipation coating, that the heat dissipation performance of the graphene heat dissipation coating is not only related to the dispersibility of graphene in a coating and the compatibility of graphene and a resin, but also the hardness of a heat conductive filler in the coating affects the heat dissipation effect of the graphene heat dissipation coating. Thereby forming the technical scheme of the invention.
A water-based graphene composite heat dissipation coating comprises a component A and a component B;
the component A comprises reduced graphene oxide slurry, water-based epoxy resin, heat-conducting filler, an auxiliary agent and water;
wherein the reduced graphene oxide slurry is prepared by thermally reducing an aqueous solution of graphene oxide;
the Mohs hardness of the heat-conducting filler is not less than 7;
the component B comprises an epoxy curing agent and water.
According to the invention, the heat-conducting filler with proper hardness is selected, and the reduced graphene oxide which has no adverse effect when matched with the heat-conducting filler and can be well dispersed in the coating and well compatible with the epoxy resin is selected, and the component A of the water-based graphene composite heat-dissipating coating is formed together with the water-based epoxy resin and water. The epoxy curing agent and water are used as the component B of the aqueous graphene composite heat dissipation coating, and compared with the traditional scheme, the aqueous graphene composite heat dissipation coating has a good heat dissipation effect.
Optionally, the preparation method of the reduced graphene oxide comprises the following steps:
and carrying out reduction reaction on the aqueous solution of the graphene oxide for 1-4 h at the temperature of 200-500 ℃ and under the pressure of 123-309 KPa.
Optionally, the method for preparing reduced graphene oxide does not include the step of adding a reducing agent.
Optionally, the mass concentration of the aqueous solution of the graphene oxide is 0.5-10%, and the amount ratio of carbon-oxygen substances in the graphene oxide is (1.2-2.0): 1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
Optionally, the thermally conductive filler is selected from alumina and/or silicon carbide.
Optionally, the particle size of the alumina is 2-20 μm, and the Mohs hardness is 8-9.5.
The particle size of the silicon carbide is 2-20 microns, and the Mohs hardness is 9-10.
Optionally, the heat conducting filler is a combination of aluminum oxide and silicon carbide, and the mass ratio of the aluminum oxide to the silicon carbide is n: (10-n), wherein n is any value excluding 10 in the range of 5-10.
Optionally, the solid content of the aqueous epoxy resin is 40% to 70%.
Optionally, the adjuvant is selected from at least one of a dispersant, a wetting agent, an aqueous rheology adjuvant, a defoamer, and a thickener.
Optionally, the dispersant is selected from at least one of carboxylate dispersants, aliphatic amide dispersants and ester dispersants.
Optionally, the wetting agent is selected from at least one of sodium dodecyl benzene sulfonate, fluorinated polyacrylate, polyoxyethylene octylphenol ether and polyoxyethylene alkyl acid ether.
Optionally, the aqueous rheological aid is selected from at least one of polyacrylic acid and polyether modified polysiloxane.
Optionally, the defoamer is selected from at least one of mineral oil and silicone.
Optionally, the thickener is selected from at least one of an acrylic-type thickener, a polyurethane-type thickener, and bentonite.
Optionally, the epoxy curing agent is selected from at least one of methylenedicyclohexylamine and isophoronediamine.
In some embodiments, the a component comprises the following preparation raw materials in parts by weight:
10-100 parts of reduced graphene oxide slurry, 200-500 parts of water-based epoxy resin, 200-450 parts of heat-conducting filler, 18-120 parts of assistant and 50-200 parts of water.
The component B comprises the following preparation raw materials in parts by weight:
50-200 parts of epoxy curing agent and 800-950 parts of water.
In some embodiments, the adjuvant comprises the following components in parts by weight:
5-20 parts of dispersing agent, 5-20 parts of wetting agent, 2-40 parts of aqueous rheological additive, 1-10 parts of defoaming agent and 5-30 parts of thickening agent.
At this time, the component A comprises the following preparation raw materials:
10-100 parts of reduced graphene oxide slurry, 200-500 parts of water-based epoxy resin, 200-450 parts of heat-conducting filler, 5-20 parts of dispersing agent, 5-20 parts of wetting agent, 2-40 parts of water-based rheological additive, 1-10 parts of defoaming agent, 5-20 parts of thickening agent and 50-200 parts of water.
The water-based graphene composite heat dissipation coating uses water as a diluent, is green and environment-friendly, and initiatively proposes that the reduced graphene oxide of the thermal reduced graphene oxide aqueous solution and the heat conduction filler with Mohs hardness not less than 7 are used together, so that the heat dissipation effect of the coating is improved.
A preparation method of a water-based graphene composite heat dissipation coating comprises the following steps:
mixing reduced graphene oxide slurry, an auxiliary agent and water, adding a heat-conducting filler for continuous mixing, adding a water-based epoxy resin for continuous mixing, and preparing a component A;
mixing an epoxy curing agent and water to prepare a component B;
and (2) mixing the component A and the component B according to the mass ratio of (8-15): 1, mixing and curing.
Optionally, the curing temperature is 80-150 ℃, and the curing time is 30 min-2 h.
Optionally, the rotation speed of the mixed reduced graphene oxide slurry, the auxiliary agent and the water is 400-1000 r/min, and the time is 5-20 min.
Optionally, the rotating speed of adding the heat-conducting filler for continuous mixing is 1500 r/min-2500 r/min, and the time is 20 min-60 min.
Optionally, the rotation speed of adding the waterborne epoxy resin for continuous mixing is 500 r/min-1000 r/min, and the time is 10 min-30 min.
Optionally, the rotating speed of the mixed epoxy curing agent and water is 200 r/min-800 r/min, and the time is 5 min-20 min.
In the following, the raw materials referred to in the following specific examples are commercially available, unless otherwise specified, the equipment used, and the processes referred to, unless otherwise specified, are all routinely selected by those skilled in the art.
Example 1
The embodiment provides a water-based graphene composite heat dissipation coating and a preparation method thereof, and the preparation method comprises the following steps:
(1) the following raw materials were prepared in the following weight parts
The component A comprises: 50 parts of reduced graphene oxide slurry, 10 parts of a dispersing agent, 5 parts of a wetting agent, 20 parts of a water-based rheological additive, 1 part of a defoaming agent, 5 parts of a thickening agent, 400 parts of water-based epoxy resin, 300 parts of a heat-conducting filler and 150 parts of water.
And B component: 150 parts of epoxy curing agent and 850 parts of water.
The preparation method of the reduced graphene oxide slurry comprises the following steps: directly reducing the aqueous solution of the graphene oxide for 3 hours at the temperature of 300 ℃ and under the pressure of 150KPa without adding any reducing agent.
The mass concentration of the aqueous solution of the graphene oxide is 2%, the quantity ratio of carbon to oxygen substances in the graphene oxide is 2.0:1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
The dispersing agent is a combination of an aliphatic amide dispersing agent and a lipid dispersing agent, and the mass ratio of the aliphatic amide dispersing agent to the lipid dispersing agent is 1: 1.
The wetting agent is alkyl acid polyoxyethylene ether.
The aqueous rheological additive is polyacrylic acid.
The defoaming agent is a combination of mineral oil and organic silicon, and the mass ratio of the mineral oil to the organic silicon is 1: 1.
The thickening agent is bentonite.
The solid content of the waterborne epoxy resin is 70%.
The heat conducting filler is a combination of aluminum oxide and silicon carbide. The particle size of the alumina was 5 μm and the particle size of the silicon carbide was 10 μm. The mass ratio of the aluminum oxide to the silicon carbide is 7: 3.
The water is deionized water.
The epoxy curing agent is methylene dicyclohexylamine.
(2) Preparation of component A
And S1, sequentially adding the reduced graphene oxide slurry, water, a dispersing agent, a wetting agent, an aqueous rheological additive, a defoaming agent and a thickening agent into a material cylinder, starting dispersing equipment, and dispersing for 10min at the rotating speed of 500 r/min.
And S2, adding the heat-conducting filler, continuously mixing, adjusting the rotating speed to 2500r/min, and dispersing for 60 min.
And S3, adjusting the rotating speed to 600r/min, adding the water-based epoxy resin, and dispersing for 10min to obtain the component A.
(3) Preparation of component B
And stirring the epoxy curing agent and water for 10min under the condition of 300r/min to obtain the component B.
(4) Curing
When in use, the component A and the component B are mixed according to the mass ratio of 10: 1. The curing temperature of the coating is 80 ℃, and the curing time is 1 h.
Example 2
The embodiment provides a water-based graphene composite heat dissipation coating and a preparation method thereof, which are basically the same as those in embodiment 1, and mainly differ in that the particle size of the heat conductive filler is different. The method comprises the following steps:
(1) the following raw materials were prepared in the following weight parts
And (2) component A: the modified graphene oxide coating comprises, by weight, 50 parts of reduced graphene oxide slurry, 10 parts of a dispersing agent, 5 parts of a wetting agent, 20 parts of a water-based rheological additive, 1 part of a defoaming agent, 5 parts of a thickening agent, 400 parts of a water-based epoxy resin, 300 parts of a heat-conducting filler and 150 parts of water.
And B component: 150 parts of epoxy curing agent and 850 parts of water.
The preparation method of the reduced graphene oxide slurry comprises the following steps: directly reducing the aqueous solution of the graphene oxide for 3 hours at the temperature of 300 ℃ and under the pressure of 150KPa without adding any reducing agent.
The mass concentration of the aqueous solution of the graphene oxide is 2%, the quantity ratio of carbon to oxygen substances in the graphene oxide is 2.0:1, the sheet diameter of the graphene oxide is 2-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
The dispersing agent is a combination of an aliphatic amide dispersing agent and a lipid dispersing agent, and the mass ratio of the aliphatic amide dispersing agent to the lipid dispersing agent is 1: 1.
The wetting agent is alkyl acid polyoxyethylene ether.
The aqueous rheological additive is polyacrylic acid.
The defoaming agent is a combination of mineral oil and organic silicon, and the mass ratio of the mineral oil to the organic silicon is 1: 1.
The thickening agent is bentonite.
The solid content of the waterborne epoxy resin is 70%.
The heat conducting filler is a combination of aluminum oxide and silicon carbide. The particle size of the alumina was 2 μm and the particle size of the silicon carbide was 5 μm. The mass ratio of the aluminum oxide to the silicon carbide is 7: 3.
The water is deionized water.
The epoxy curing agent is methylene dicyclohexylamine.
(2) Preparation of component A
And S1, sequentially adding the reduced graphene oxide slurry, water, a dispersing agent, a wetting agent, an aqueous rheological additive, a defoaming agent and a thickening agent into a material cylinder, starting dispersing equipment, and dispersing for 10min at the rotating speed of 500 r/min.
And S2, adding the heat-conducting filler, continuously mixing, adjusting the rotating speed to 2500r/min, and dispersing for 60 min.
And S3, adjusting the rotating speed to 600r/min, adding the water-based epoxy resin, and dispersing for 10min to obtain the component A.
(3) Preparation of the B component
And stirring the epoxy curing agent and water for 10min under the condition of 300r/min to obtain the component B.
(4) Curing
When in use, the component A and the component B are mixed according to the mass ratio of 10: 1. The curing temperature of the coating is 80 ℃, and the curing time is 1 h.
Example 3
The embodiment provides an aqueous graphene composite heat dissipation coating and a preparation method thereof, and the main difference from embodiment 1 is that the preparation raw materials, the amounts and the preparation methods of the component a and the component B are different. The method comprises the following steps:
(1) the following raw materials were prepared in the following weight parts
The component A comprises: 80 parts of reduced graphene oxide slurry, 15 parts of dispersing agent, 20 parts of wetting agent, 30 parts of aqueous rheological additive, 5 parts of defoaming agent, 30 parts of thickening agent, 300 parts of aqueous epoxy resin, 350 parts of heat-conducting filler and 160 parts of water.
And B component: 80 parts of epoxy curing agent and 920 parts of water.
The preparation method of the reduced graphene oxide slurry comprises the following steps: directly reducing the aqueous solution of the graphene oxide for 2h at the temperature of 280 ℃ and the pressure of 250KPa without adding any reducing agent.
The mass concentration of the aqueous solution of the graphene oxide is 5%, the quantity ratio of carbon to oxygen substances in the graphene oxide is 1.2:1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
The dispersant is a carboxylate dispersant.
The wetting agent is octyl phenol polyoxyethylene ether.
The aqueous rheological additive is polyether modified polysiloxane.
The defoaming agent is mineral oil.
The thickener is an acrylic acid type thickener.
The solid content of the waterborne epoxy resin is 60%.
The heat conducting filler is a combination of aluminum oxide and silicon carbide. The particle size of the alumina was 10 μm and the particle size of the silicon carbide was 5 μm. The mass ratio of alumina to silicon carbide was 6: 4.
The water is deionized water.
The epoxy curing agent is isophorone diamine.
(2) Preparation of component A
And S1, sequentially adding the reduced graphene oxide slurry, water, a dispersing agent, a wetting agent, an aqueous rheological additive, a defoaming agent and a thickening agent into a material cylinder, starting dispersing equipment, and dispersing for 15min at the rotating speed of 600 r/min.
And S2, adding the heat-conducting filler, continuously mixing, adjusting the rotating speed to 2300r/min, and dispersing for 30min.
And S3, adjusting the rotating speed to 600r/min, adding the water-based epoxy resin, and dispersing for 20min to obtain the component A.
(3) Preparation of component B
And stirring the epoxy curing agent and water for 20min under the condition of 500r/min to obtain the component B.
(4) Curing
When the paint is used, the component A and the component B are mixed according to the mass ratio of 15: 1. The curing temperature of the coating is 100 ℃, and the curing time is 30min.
Example 4
The embodiment provides a water-based graphene composite heat dissipation coating and a preparation method thereof, and the main difference from embodiment 1 is that the preparation raw materials, the use amounts and the preparation methods of the component a and the component B are different. The method comprises the following steps:
(1) the following raw materials were prepared in the following weight parts
The component A comprises: 100 parts of reduced graphene oxide slurry, 20 parts of dispersing agent, 5 parts of wetting agent, 10 parts of aqueous rheological additive, 2 parts of defoaming agent, 5 parts of thickening agent, 380 parts of aqueous epoxy resin, 250 parts of heat-conducting filler and 180 parts of water.
And B component: 200 parts of epoxy curing agent and 800 parts of water.
The preparation method of the reduced graphene oxide slurry comprises the following steps: directly reducing the aqueous solution of the graphene oxide for 2.5h at the temperature of 400 ℃ and the pressure of 150KPa without adding any reducing agent.
The mass concentration of the aqueous solution of the graphene oxide is 1%, the quantity ratio of carbon to oxygen substances in the graphene oxide is 1.5:1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
The dispersant is a carboxylate dispersant.
The wetting agent is octyl phenol polyoxyethylene ether.
The aqueous rheological additive is a combination of polyacrylic acid and polyether modified polysiloxane, and the mass ratio of the polyacrylic acid to the polyether modified polysiloxane is 2: 1.
The defoaming agent is organic silicon.
The thickener is an acrylic acid type thickener.
The solid content of the waterborne epoxy resin is 65%.
The heat conducting filler is a combination of aluminum oxide and silicon carbide. The particle size of the alumina was 2 μm and the particle size of the silicon carbide was 10 μm. The mass ratio of the alumina to the silicon carbide is 8: 2.
The water is deionized water.
The epoxy curing agent is a combination of methylene dicyclohexyl amine and isophorone diamine, and the mass ratio of the methylene dicyclohexyl amine to the isophorone diamine is 1: 1.
(2) Preparation of component A
And S1, sequentially adding the reduced graphene oxide slurry, water, a dispersing agent, a wetting agent, an aqueous rheological additive, a defoaming agent and a thickening agent into a material cylinder, starting dispersing equipment, and dispersing for 10min at the rotating speed of 1000 r/min.
And S2, adding the heat-conducting filler, continuously mixing, adjusting the rotating speed to 2500r/min, and dispersing for 50 min.
And S3, adjusting the rotating speed to 500r/min, adding the water-based epoxy resin, and dispersing for 30min to obtain the component A.
(3) Preparation of component B
And stirring the epoxy curing agent and water for 20min under the condition of 1000r/min to obtain the component B.
(4) Curing
When the paint is used, the mass ratio of the component A to the component B is 20: 1. The curing temperature of the coating is 70 ℃, and the curing time is 40 min.
Comparative example 1
The comparative example provides a water-based graphene composite heat dissipation coating and a preparation method thereof, which are basically the same as those in example 4, and mainly differ in that the heat-conducting filler uses BN (boron nitride) with the particle size of 3 microns and the Mohs hardness of 2. The method comprises the following steps:
(1) the following raw materials were prepared in the following weight parts
The component A comprises: 100 parts of reduced graphene oxide slurry, 20 parts of dispersing agent, 5 parts of wetting agent, 10 parts of aqueous rheological additive, 2 parts of defoaming agent, 5 parts of thickening agent, 380 parts of aqueous epoxy resin, 250 parts of heat-conducting filler and 180 parts of water.
And B component: 200 parts of epoxy curing agent and 800 parts of water.
The preparation method of the reduced graphene oxide slurry comprises the following steps: directly reducing the aqueous solution of the graphene oxide for 2.5h at the temperature of 400 ℃ and under the pressure of 150KPa without adding any reducing agent.
The mass concentration of the aqueous solution of the graphene oxide is 1%, the quantity ratio of carbon to oxygen substances in the graphene oxide is 1.5:1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
The dispersant is a carboxylate dispersant.
The wetting agent is octyl phenol polyoxyethylene ether.
The aqueous rheological additive is a combination of polyacrylic acid and polyether modified polysiloxane, and the mass ratio of the polyacrylic acid to the polyether modified polysiloxane is 2: 1.
The defoaming agent is organic silicon.
The thickener is an acrylic acid type thickener.
The solid content of the waterborne epoxy resin is 65%.
The heat-conducting filler is BN. BN had a particle size of 3 μm and a Mohs hardness of 2.
The water is deionized water.
The epoxy curing agent is a combination of methylene dicyclohexyl amine and isophorone diamine, and the mass ratio of the methylene dicyclohexyl amine to the isophorone diamine is 1: 1.
(2) Preparation of component A
And S1, sequentially adding the reduced graphene oxide slurry, water, a dispersing agent, a wetting agent, an aqueous rheological additive, a defoaming agent and a thickening agent into a material cylinder, starting dispersing equipment, and dispersing for 10min at the rotating speed of 1000 r/min.
And S2, adding the heat-conducting filler, continuously mixing, adjusting the rotating speed to 2500r/min, and dispersing for 50 min.
And S3, adjusting the rotating speed to 500r/min, adding the water-based epoxy resin, and dispersing for 30min to obtain the component A.
(3) Preparation of component B
And stirring the epoxy curing agent and water for 20min under the condition of 1000r/min to obtain the component B.
(4) Curing of
When in use, the component A and the component B are mixed according to the mass ratio of 20: 1. The curing temperature of the coating is 70 ℃, and the curing time is 40 min.
Comparative example 2
The comparative example provides a water-based graphene composite heat dissipation coating and a preparation method thereof, which are basically the same as those in example 4, and mainly differ in that reduced graphene oxide slurry is replaced by reduced graphene oxide prepared by other methods. The method comprises the following steps:
(1) the following raw materials were prepared in the following weight parts
The component A comprises: 100 parts of reduced graphene oxide slurry, 20 parts of dispersing agent, 5 parts of wetting agent, 10 parts of aqueous rheological additive, 2 parts of defoaming agent, 5 parts of thickening agent, 380 parts of aqueous epoxy resin, 250 parts of heat-conducting filler and 180 parts of water.
And B component: 200 parts of epoxy curing agent and 800 parts of water.
The preparation method of the reduced graphene oxide slurry comprises the following steps: adding a hydrazine hydrate solution into an aqueous solution of graphene oxide, and reacting for 8 hours at 100 ℃ to obtain reduced graphene oxide slurry with the carbon content of more than 95%.
The mass concentration of the aqueous solution of the graphene oxide is 1%, the quantity ratio of carbon to oxygen substances in the graphene oxide is 1.5:1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
The dispersant is a carboxylate dispersant.
The wetting agent is octyl phenol polyoxyethylene ether.
The aqueous rheological additive is a combination of polyacrylic acid and polyether modified polysiloxane, and the mass ratio of the polyacrylic acid to the polyether modified polysiloxane is 2: 1.
The defoaming agent is organic silicon.
The thickener is an acrylic acid type thickener.
The solid content of the waterborne epoxy resin is 65%.
The heat conducting filler is a combination of aluminum oxide and silicon carbide. The particle size of the alumina was 2 μm and the particle size of the silicon carbide was 10 μm. The mass ratio of the alumina to the silicon carbide is 8: 2.
The water is deionized water.
The epoxy curing agent is a combination of methylene dicyclohexyl amine and isophorone diamine, and the mass ratio of the methylene dicyclohexyl amine to the isophorone diamine is 1: 1.
(2) Preparation of component A
And S1, sequentially adding the reduced graphene oxide slurry, water, a dispersing agent, a wetting agent, an aqueous rheological additive, a defoaming agent and a thickening agent into a material cylinder, starting dispersing equipment, and dispersing for 10min at the rotating speed of 1000 r/min.
And S2, adding the heat-conducting filler, continuously mixing, adjusting the rotating speed to 2500r/min, and dispersing for 50 min.
And S3, adjusting the rotating speed to 500r/min, adding the water-based epoxy resin, and dispersing for 30min to obtain the component A.
(3) Preparation of component B
And stirring the epoxy curing agent and water for 20min under the condition of 1000r/min to obtain the component B.
(4) Curing
When in use, the component A and the component B are mixed according to the mass ratio of 20: 1. The curing temperature of the coating is 70 ℃, and the curing time is 40 min.
The coatings of the above examples and comparative examples were cured under the same device substrate to form a coating, and the heat dissipation effect was examined as follows:
the heat dissipation effect is as follows: the temperature difference of the test device under the conditions of heating power of 20W and heating time of 1h under the condition of no coating or the condition of coating is compared, and the temperature difference of each embodiment and each comparative example is compared.
TABLE 1
As can be seen from table 1, the hardness of the thermal conductive filler has an influence on the heat dissipation effect of the device when a subsequent coating is formed, and meanwhile, after the thermal conductive filler with appropriate hardness is added, the requirement is placed on the preparation method of the reduced graphene oxide slurry, and the reduced graphene oxide obtained by the method of thermally reducing the aqueous solution of graphene oxide has relatively low carbon content and good hydrophilicity, and can act together with the thermal conductive filler with appropriate hardness to improve the heat dissipation effect of the coating.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The water-based graphene composite heat dissipation coating is characterized by comprising a component A and a component B;
the component A comprises reduced graphene oxide slurry, water-based epoxy resin, heat-conducting filler, an auxiliary agent and water;
wherein the reduced graphene oxide slurry is prepared by thermally reducing an aqueous solution of graphene oxide;
the Mohs hardness of the heat-conducting filler is not less than 7;
the component B comprises an epoxy curing agent and water.
2. The aqueous graphene composite heat dissipation coating as recited in claim 1, wherein the preparation method of the reduced graphene oxide comprises the following steps:
and carrying out reduction reaction on the aqueous solution of the graphene oxide for 1-4 h at the temperature of 200-500 ℃ and under the pressure of 123-309 KPa.
3. The water-based graphene composite heat dissipation coating as claimed in claim 2, wherein the mass concentration of the aqueous solution of graphene oxide is 0.5-10%, and the amount ratio of carbon-oxygen substances in the graphene oxide is (1.2-2.0): 1, the sheet diameter of the graphene oxide is 1-50 mu m, and the thickness of the graphene oxide is 1-3 nm.
4. The aqueous graphene composite heat dissipation coating of claim 1, wherein the thermally conductive filler is selected from alumina and/or silicon carbide.
5. The water-based graphene composite heat dissipation coating as claimed in claim 4, wherein the particle size of the aluminum oxide is 2 μm to 20 μm; and/or
The grain diameter of the silicon carbide is 2-20 mu m; and/or
The heat conducting filler is a combination of aluminum oxide and silicon carbide, and the mass ratio of the aluminum oxide to the silicon carbide is n: (10-n), wherein n is any value excluding 10 in the range of 5-10.
6. The water-based graphene composite heat dissipation coating as claimed in any one of claims 1 to 5, wherein the solid content of the water-based epoxy resin is 40% to 70%; and/or
The auxiliary agent is at least one selected from a dispersing agent, a wetting agent, an aqueous rheological auxiliary agent, a defoaming agent and a thickening agent.
7. The aqueous graphene composite heat dissipation coating of claim 6, wherein the dispersant is at least one selected from a carboxylate dispersant, an aliphatic amide dispersant and an ester dispersant; and/or
The wetting agent is selected from at least one of sodium dodecyl benzene sulfonate, fluorinated polyacrylate, polyoxyethylene octylphenol ether and polyoxyethylene alkyl acid ether; and/or
The aqueous rheological additive is selected from at least one of polyacrylic acid and polyether modified polysiloxane; and/or
The defoaming agent is at least one of mineral oil and organic silicon; and/or
The thickening agent is selected from at least one of acrylic thickening agent, polyurethane thickening agent and bentonite; and/or
The epoxy curing agent is at least one selected from methylene dicyclohexyl amine and isophorone diamine.
8. The water-based graphene composite heat dissipation coating as recited in any one of claims 1 to 5, wherein the component A comprises the following preparation raw materials in parts by weight:
10-100 parts of reduced graphene oxide slurry, 200-500 parts of water-based epoxy resin, 200-450 parts of heat-conducting filler, 18-120 parts of assistant and 50-200 parts of water;
the component B comprises the following preparation raw materials in parts by weight:
50-200 parts of epoxy curing agent and 800-950 parts of water.
9. A preparation method of a water-based graphene composite heat dissipation coating is characterized by comprising the following steps:
mixing reduced graphene oxide slurry, an auxiliary agent and water, adding a heat-conducting filler for continuous mixing, adding a water-based epoxy resin for continuous mixing, and preparing a component A;
mixing an epoxy curing agent and water to prepare a component B;
and (2) mixing the component A and the component B according to the mass ratio of (8-15): 1, mixing and curing.
10. The preparation method of the water-based graphene composite heat dissipation coating according to claim 9, wherein the curing temperature is 80-150 ℃, and the curing time is 30 min-2 h.
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| CN118271934A (en) * | 2024-04-22 | 2024-07-02 | 深圳职业技术大学 | Heat-conducting antibacterial nano titanium dioxide/graphene oxide modified waterborne epoxy coating for electronic packaging and preparation method thereof |
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| CN113480875A (en) * | 2021-07-27 | 2021-10-08 | 雷索新材料(苏州)有限公司 | Aluminum oxide modified graphene, graphene heat dissipation coating and preparation method thereof |
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| CN104804618A (en) * | 2014-01-24 | 2015-07-29 | 江苏联科纳米科技有限公司 | Aqueous heat dissipation coating and preparation method thereof |
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