CN116676000A - Heat dissipation coating, preparation method thereof and heating device - Google Patents
Heat dissipation coating, preparation method thereof and heating device Download PDFInfo
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- CN116676000A CN116676000A CN202310681770.6A CN202310681770A CN116676000A CN 116676000 A CN116676000 A CN 116676000A CN 202310681770 A CN202310681770 A CN 202310681770A CN 116676000 A CN116676000 A CN 116676000A
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Classifications
-
- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The application provides a heat dissipation coating, a preparation method thereof and a heating device, wherein the heat dissipation coating comprises 40-60 parts by mass of ceramic resin, based on 100 parts by mass of the total heat dissipation coating, of a dispersing agent, a filler and a solvent. The heat-dissipating coating has the characteristics of high temperature resistance, excellent heat dissipation performance and good durability.
Description
Technical Field
The application relates to the technical field of heat dissipation, in particular to a heat dissipation coating, a preparation method thereof and a heating device.
Background
The graphene has good electric conduction and heat conduction properties, and compared with an aluminum sheet material, the graphene has the electric energy conversion rate of more than 99 percent, good thermal stability and high heating efficiency. The thermal conductivity of the defect-free single-layer graphene is as high as 5300W/(m.K), which is higher than that of single-wall carbon nanotubes and multi-wall carbon nanotubes.
The fin type electric heating tube has less than 10% of infrared radiant energy, most of the infrared radiant energy is heat energy conduction, the heat conductivity of air is low, the convection heat transfer coefficient is low, and therefore the heat transfer efficiency is low. In addition, the fin type electric heating pipe is low in heat dissipation, so that the space temperature rise is low, and a common solution is to add an air supply system to enable air on the surface of the fin type electric heating pipe to flow, however, the addition of the air supply system not only increases the volume and the weight of equipment, but also increases the material cost and the electricity cost.
In the prior art, by spraying heat dissipation materials on the surface of the fin type electric heating pipe, heat conduction and infrared radiation energy are improved, and under the action of a dual heating principle, the heated object is heated more quickly, and absorbed heat energy is more sufficient. The infrared heating emitted by the graphene heat dissipation does not harm human body, and the infrared heating appears in a form of 6-14 mu m far infrared light wave physiotherapy heating, and is easy to be absorbed and converted by the human body when contacting with the human body, so that the comfort is improved.
However, the graphene coating has the problems of poor binding force and poor stability, so how to provide a heat dissipation coating capable of ensuring the binding force and the stability of the coating is a technical problem which needs to be solved urgently at present.
Disclosure of Invention
Based on the above, it is necessary to provide a heat-dissipating coating, a preparation method thereof and a heating device, which solve the problems of slow heat transfer and high energy consumption of a heater in a high temperature state (500 ℃), and the heat-dissipating coating of the present application has the characteristics of high temperature resistance, excellent heat dissipation and good durability.
The above object can be achieved by the following technical scheme.
In a first aspect, the application provides a heat-dissipating coating, which comprises 40-60 parts by weight of ceramic resin, based on 100 parts by weight of the total heat-dissipating coating, of ceramic resin, graphene, a dispersing agent, a filler and a solvent.
In some embodiments, the heat-dissipating coating satisfies at least one of the following conditions, based on 100 parts of the total mass of the heat-dissipating coating:
(1) The mass portion of the graphene is 3-12
(2) The mass part of the dispersing agent is 1-2;
(3) The mass portion of the filler is 20-30;
(4) The mass portion of the solvent is 10-20.
In some embodiments, the ceramic resin comprises an oxide sol-type ceramic resin.
In some embodiments, the oxide sol-based ceramic resin includes at least one of a silica sol, an alumina sol, a colloidal zirconia sol, a ceria sol, and a nickel oxide sol.
In some embodiments, the number of layers of graphene is 1 to 20.
In some embodiments, the graphene has a particle size D50 < 6 μm.
In some embodiments, the graphene comprises at least one of graphene oxide, reduced graphene oxide, and doped graphene.
In some embodiments, the dispersant comprises at least one of an ammonium carboxylate salt, a polyester phosphate ester, and a polycaprolactone polyurethane.
In some embodiments, the dispersant has a molecular weight of 2000 to 3000.
In some embodiments, the filler comprises at least one of mica powder and talc.
In some embodiments, the filler has a diameter of 400 mesh to 600 mesh.
In some embodiments, the heat-dissipating coating further comprises an auxiliary agent. Optionally, the auxiliary agent comprises at least one of a coupling agent, an acidity regulator, a thixotropic agent and a leveling agent.
In some embodiments, the coupling agent comprises a silane coupling agent.
Optionally, the coupling agent is 2-5 parts based on 100 parts of the total mass of the heat dissipation coating.
In some embodiments, the acidity regulator comprises at least one of acetic acid and lactic acid.
Optionally, the acid regulator is 0.1 to 1 part based on 100 parts of the total mass of the heat dissipation coating.
In some embodiments, the thixotropic agent comprises fumed silica.
Optionally, the thixotropic agent is 1 to 3 parts based on 100 parts of the total mass of the heat dissipation coating.
In some embodiments, the leveling agent comprises a silicone leveling agent.
Optionally, the leveling agent is 0.1 to 1 part based on 100 parts of the total mass of the heat dissipation coating.
In a second aspect, the present application provides a method for preparing the heat-dissipating coating according to the first aspect, the method comprising:
and mixing ceramic resin, graphene, a dispersing agent, a filler and a solvent to prepare the heat dissipation coating.
In some embodiments, the heat-dissipating coating further comprises an auxiliary agent, optionally comprising at least one of a coupling agent, an acidity regulator, a thixotropic agent, and a leveling agent, the preparation method comprising:
mixing ceramic resin, a coupling agent, an acid regulator, a dispersing agent, a leveling agent and a solvent, and then adding a filler, a thixotropic agent and graphene for mixing to prepare the heat dissipation coating.
In a third aspect, the present application provides a heat-generating device comprising a heat-dissipating layer prepared from a heat-dissipating coating comprising the heat-dissipating coating of the first aspect.
Compared with the prior art, the application has at least the following beneficial effects:
the application adopts ceramic resin, graphene, dispersing agent and filler, so that the coating has film forming property and high temperature resistance, has good adhesive force to metal and ceramic, belongs to high temperature fusion in the process of forming a coating by spraying and sintering, and the ceramic resin at the interface of the coating is tightly combined with a radiator, so that the adhesive force is not deteriorated even if the ceramic resin is put into cold water under the high temperature condition for cooling, and the application has the characteristics of convenient use, long storage period, good stability and the like.
Detailed Description
The following detailed description of the present application is provided merely to illustrate the application and is not intended to limit the scope of the application in any way, in connection with the embodiments and examples which are provided to provide a more thorough understanding of the present disclosure. It will also be appreciated that the present application may be embodied in many different forms and is not limited to the embodiments and examples described herein, but may be modified or altered by persons skilled in the art without departing from the spirit of the application, and equivalents thereof are also intended to fall within the scope of the application. Furthermore, in the following description, numerous specific details are set forth in order to provide a more thorough understanding of the application, it being understood that the application may be practiced without one or more of these details.
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 application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
In the present application, "optional" means optional or not, that is, means any one selected from two parallel schemes of "with" or "without". If multiple "alternatives" occur in a technical solution, if no particular description exists and there is no contradiction or mutual constraint, then each "alternative" is independent.
In the present application, the terms "first", "second", "third", etc. are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity, nor as implying an importance or quantity of a technical feature being indicated. Moreover, "first," "second," "third," etc. are for non-exhaustive list description purposes only, and it should be understood that no closed limitation on the number is made.
In the application, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present application, a numerical range (i.e., a numerical range) is referred to, and, unless otherwise indicated, a distribution of optional values within the numerical range is considered to be continuous and includes two numerical endpoints (i.e., a minimum value and a maximum value) of the numerical range, and each numerical value between the two numerical endpoints. When a numerical range merely points to integers within the numerical range, unless expressly stated otherwise, both endpoints of the numerical range are inclusive of the integer between the two endpoints, and each integer between the two endpoints is equivalent to the integer directly recited. When multiple numerical ranges are provided to describe a feature or characteristic, the numerical ranges may be combined. In other words, unless otherwise indicated, the numerical ranges disclosed in this application are to be understood to include any and all subranges subsumed therein. The "numerical value" in the numerical interval may be any quantitative value, such as a number, a percentage, a proportion, or the like. "numerical interval" allows to broadly include quantitative intervals such as percentage intervals, proportion intervals, ratio intervals, etc.
In the traditional technology, epoxy resin, polyester resin, acrylic resin and graphene materials are mixed to be used as a coating, but the materials are mainly formed by a large number of-C-C-, -C-O-, and-N-C-, and the like, so that the bond energy is low, the coating is not ageing-resistant, the highest softening temperature is lower than 200 ℃, namely the heating temperature is higher than 200 ℃, the coating loses cohesiveness, and even the coating is oxidized and yellow or powdered in the air; further, when the heating temperature is higher than 250 ℃, severe oxidation reaction is carried out to completely decompose, and harmful gases (such as CO, NO and the like) are generated; and the coating becomes brittle and cracks under the environment of 0 ℃ and the binding force is reduced. Therefore, the heat dissipation paint in the conventional technology cannot meet the high and low temperature environmental requirements. The application adopts ceramic resin, dispersant and filler, so that the graphene heat dissipation coating has good film forming property and excellent high temperature resistance and oxidation resistance.
The first aspect of the application provides a heat-dissipating coating, which comprises 40-60 parts by weight of ceramic resin, based on 100 parts by weight of the total heat-dissipating coating, of ceramic resin, graphene, a dispersing agent, a filler and a solvent.
According to the application, graphene, ceramic resin, a dispersing agent and a filler are adopted to form the heat-dissipating coating, so that the coating is stable, a high-temperature-resistant coating can be formed, and the heat conductivity can be improved by converting radiation into heat; the film layer after forming the coating is compact, does not contain organic combustibles, and has excellent high temperature resistance (not more than 600 ℃), oxidation resistance, flame resistance, ultraviolet resistance and ozone corrosion resistance.
For example, the ceramic resin may be, but is not limited to, 40 parts, 42 parts, 44 parts, 46 parts, 48 parts, 50 parts, 52 parts, 54 parts, 56 parts, 58 parts, 60 parts, or a range between any two of the foregoing.
The ceramic resin has the main component of inorganic ceramic material sol, is an inorganic film forming material, does not contain combustible substances after solidification, and has high temperature resistance.
In some embodiments, the mass portion of the graphene is 3 to 12 parts based on 100 parts of the total mass of the heat dissipating coating, for example, the graphene may be, but not limited to, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, or a range between any two of the above.
In some embodiments, the dispersant is 1 to 2 parts by mass based on 100 parts by mass of the heat dissipating coating, for example, the dispersant may be 1.0 part, 1.1 part, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 19 parts, or 2.0 parts.
In some embodiments, the filler is 20 parts to 30 parts by mass based on 100 parts by mass of the total heat dissipating coating, for example, the filler may be 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, or 30 parts.
In some embodiments, the solvent is 10 parts to 20 parts by mass based on 100 parts by mass of the total heat dissipating coating, for example, the solvent may be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, or 20 parts.
In some embodiments, the ceramic resin comprises an oxide sol-type ceramic resin.
In some embodiments, the oxide sol-based ceramic resin includes at least one of a silica sol, an alumina sol, a colloidal zirconia sol, a ceria sol, and a nickel oxide sol. Silica sols and alumina sols are preferred.
In some implementations, the ceramic resin has a solids content of 20% to 40%.
In some implementations, the ceramic resin has a viscosity of 30cps to 100cps.
In some implementations, the ceramic resin has a pH of 4 to 5.
In some embodiments, the graphene has 1 to 20 layers, for example 1, 2, 4, 6, 8, 10, 12, 14, 16, 18, or 20 layers.
In some embodiments, the graphene has a particle size D50 < 6 μm, for example 0.5 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, or 6 μm.
In some embodiments, the graphene comprises at least one of graphene oxide, reduced graphene oxide, and doped graphene.
In some embodiments, the dispersant includes at least one of an ammonium carboxylate salt, a polyester phosphate ester, and a polycaprolactone polyurethane.
In some embodiments, the dispersant has a molecular weight of 2000 to 3000. For example 2000, 2100, 2200, 2300, 2400, 2500, 2600, 2700, 2800, 2900 or 3000.
According to the application, small molecular (with molecular weight of 2000-3000) ammonium carboxylate is used as a dispersing agent, so that the dispersibility and stability of graphene powder in the coating can be ensured, the deflocculating and anti-settling effects can be improved, the adding amount of graphene is increased, the viscosity of the coating is reduced, and the problems of agglomeration and flocculation of the dispersed graphene are effectively prevented from affecting the spraying property of the coating and the heat dissipation property of the dry film.
In some embodiments, the filler comprises at least one of mica powder and talc. According to the application, by adding mica, which is a platy filler, the curing shrinkage can be reduced, and the waterproof effect is achieved.
In some embodiments, the filler has a diameter of 400 mesh to 600 mesh, for example 400 mesh, 420 mesh, 440 mesh, 460 mesh, 480 mesh, 500 mesh, 520 mesh, 540 mesh, 560 mesh, 580 mesh, or 600 mesh.
In some embodiments, the solvent comprises at least one of xylene and butyl acetate. The application can adjust the composition of the solvent, thereby leading the solvent to have different volatilization speeds and adjusting the drying time of the coating.
In some embodiments, the auxiliary agent includes at least one of a coupling agent, an acidity regulator, a thixotropic agent, and a leveling agent.
In some embodiments, the coupling agent comprises a silane coupling agent.
The application adopts the silane coupling agent, and for the metal material, the silane coupling agent has Si-O-R group which reacts with hydroxyl on the surface of the metal material, and also has epoxy group, amino group, sulfhydryl group and the like which are combined with film forming material, so that the adhesive force between the coating and the substrate can be improved.
Alternatively, the coupling agent is 2 to 5 parts, for example, 2.0 parts, 2.3 parts, 2.6 parts, 2.9 parts, 3.2 parts, 3.5 parts, 3.8 parts, 4.1 parts, 4.4 parts, 4.7 parts, or 5.0 parts based on 100 parts by total mass of the heat dissipating coating.
In some embodiments, the acidity regulator comprises at least one of acetic acid and lactic acid.
In the application, acetic acid and lactic acid are selected as acid regulators to stabilize the stability of the ceramic resin, so that the pH of the coating can be ensured, and the acetic acid and the lactic acid can be completely volatilized and removed in the drying process without affecting the performance of the coating.
Alternatively, the acid regulator is 0.1 to 1 part, for example, 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, or 1.0 part, based on 100 parts by total mass of the heat dissipating coating.
In some embodiments, the thixotropic agent comprises fumed silica.
The application adopts the fumed silica as the thixotropic agent, provides low shear viscosity and high shear thinning performance, improves the anti-settling property and anti-sagging property of the paint, namely has the function of improving the viscosity of the paint and preventing the paint from settling when the paint is kept stand; when the coating is formed into a coating, the viscosity is reduced, and the coating is spread.
Optionally, the saidThe specific surface area of the fumed silica is 200-400 m 2 And/g. Preferably 300m 2 /g。
Alternatively, the thixotropic agent is 1 to 3 parts, for example, 1.0 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2.0 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts or 3.0 parts based on 100 parts by total mass of the heat dissipating coating.
In some embodiments, the leveling agent comprises a silicone leveling agent.
The application adopts the organosilicon leveling agent, which has the temperature resistance of 150-200 ℃, and the volatilization in the film forming process effectively ensures the flatness of the coating, and can be decomposed in three minutes when reaching 400 ℃, compared with the acrylic leveling agent, the smell is small and no smoke is generated, and the acrylic leveling agent can generate smoke and has large taste at 400 ℃ and the volatilization time exceeds 5 minutes.
Alternatively, the leveling agent is 0.1 to 1 part, for example, 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, or 1.0 part, based on 100 parts by total mass of the heat dissipating coating.
In some embodiments, the heat-dissipating coating comprises, based on 100 parts by mass of the total mass of the heat-dissipating coating:
in a second aspect, the present application provides a method for preparing the heat-dissipating coating according to the first aspect, the method comprising:
and mixing ceramic resin, graphene, a dispersing agent, a filler and a solvent to prepare the heat dissipation coating.
In some embodiments, the heat-dissipating coating further comprises an auxiliary agent, optionally comprising at least one of a coupling agent, an acidity regulator, a thixotropic agent, and a leveling agent, the preparation method comprising:
mixing ceramic resin, a coupling agent, an acid regulator, a dispersing agent, a leveling agent and a solvent, and then adding a filler, a thixotropic agent and graphene to prepare the heat dissipation coating.
In some embodiments, during the mixing of the ceramic resin, the coupling agent, the acid regulator, the dispersant, the leveling agent, and the solvent, the stirring speed is 800r/min to 1000r/min, and the stirring time is 8min to 12min.
In some embodiments, the stirring speed is 500r/min to 600r/min during the mixing process of adding the filler, thixotropic agent and graphene.
In some embodiments, the stirring speed is 2000r/min to 2500r/min and the stirring time is 25min to 35min after the addition of the filler, thixotropic agent and graphene is completed.
In some implementations, the heat sink coating after mixing is filtered. Optionally, the filtering treatment adopts filter cloth with 50-150 meshes for filtering.
Illustratively, a method for preparing the heat dissipation coating is provided, which comprises the following steps:
mixing ceramic resin, a coupling agent, a dispersing agent, an acid regulator, a leveling agent and a solvent, and mixing for 8-12 min at a stirring speed of 800-1000 r/min to obtain a premix;
adding filler, thixotropic agent and graphene into the premix at the stirring speed of 500-600 r/min, mixing for 25-35 min at the stirring speed of 2000-2500 r/min after the addition, and filtering with filter cloth of 50-150 meshes after the stirring is completed to obtain the heat-dissipating paint.
A third aspect of the present application provides a heat dissipation layer formed from a heat dissipation coating comprising the heat dissipation coating of the first aspect.
In some embodiments, the method for preparing the heat dissipation layer includes: and coating the heat dissipation coating on the surface of the substrate, and drying to obtain the heat dissipation layer.
Optionally, the coating mode includes at least one of spraying, knife coating and spin coating.
Optionally, the drying process includes: firstly, placing for 15-20 min at room temperature, and then baking for 20-30 min at 200-260 ℃. Wherein, the room temperature is 10-35 ℃.
In a fourth aspect, the present application provides a heat generating device comprising the heat dissipation layer of the third aspect.
In some embodiments, the heat generating device comprises a finned heating tube, and the heat dissipating layer is disposed on a surface of the finned heating tube.
In some embodiments, the heat dissipation layer has a thickness of 20 μm to 30 μm.
Embodiments of the present application will be described in detail below with reference to examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. The experimental methods in the following examples, in which specific conditions are not noted, are preferably referred to the guidelines given in the present application, and may be according to the experimental manual or conventional conditions in the art, the conditions suggested by the manufacturer, or the experimental methods known in the art.
Ceramic resins are available from Sanjin pigment Limited of Zhiyang county under the designations SJ-1016 (25% solids), SJ-140M (40% solids) and SJ-482 (35% solids), respectively.
Silane coupling agents are available from Shandong Usoxhlet chemical engineering Co., ltd under the designations KH-550 (3-aminopropyl triethoxysilane), KH-560 (3-glycidoxy trimethoxysilane), KH-570 (gamma- (methacryloyloxy) propyl trimethoxysilane), KH-580 (3-mercaptopropyl trimethoxysilane) and KH-590 (3-mercaptopropyl triethoxysilane), respectively.
Xylenes were purchased from shandongtaixi chemical company.
Butyl acetate was purchased from shandongtaixi chemical company.
Acetic acid was purchased from shandongtaixi chemical company.
Leveling agents are available from BYK-333 of Pick chemistry, di Gao 450 of Yingchang chemistry and Di Gao 410 of Yingchang chemistry.
The dispersant was purchased from SN-2001 in deep bamboo chemical industry.
The filler was purchased from Anhui Gray New Material technology Co., ltd., 500 mesh mica powder.
Thixotropic agent was purchased from Degussa A30, a winning chemical group0, a specific surface area of 300m 2 Fumed silica/g.
Less graphene is purchased from LN-F of Shanghai Lishi nano technology Co., ltd, the number of layers is less than 3, and the particle size is D50 less than 6 mu m; the multilayer graphene is purchased from GP550 of fertilizer-synthesizing microcrystalline material science and technology Co-Ltd, the number of layers is 10-20, and the particle size is D50 < 6 mu m.
Example 1
Weighing raw materials according to parts by weight, including:
mixing ceramic resin, a coupling agent, a dispersing agent, an acid regulator, a leveling agent and a solvent, and mixing for 10min at a stirring speed of 9000r/min to obtain a premix;
adding filler, thixotropic agent and graphene into the premix at a stirring speed of 550r/min, mixing for 30min at a stirring speed of 2300r/min after the addition, and filtering with a 100-mesh filter cloth after the stirring is completed to obtain the heat-dissipating coating.
Example 2
A heat-dissipating coating was prepared in the same manner as in example 1 except that the ceramic resin SJ-140M in the raw material was 51.3 parts and the low-layer graphene LN-F was 9 parts.
Example 3
A heat-dissipating coating was prepared in the same manner as in example 1 except that the ceramic resin SJ-140M in the raw material was 54.3 parts and the low-layer graphene LN-F was 6 parts.
Example 4
A heat-dissipating coating was prepared as in example 1, except that 48.3 parts of ceramic resin SJ-140M was used as the starting material; the LN-F of the few-layer graphene is 12 parts.
Example 5
A heat-dissipating coating was prepared according to the method of example 1, except that few graphene layers in the raw material were replaced with the same mass fraction of multilayer graphene GP550.
Example 6
A heat-dissipating coating was prepared according to the method of example 2, except that few graphene layers in the raw material were replaced with the same mass fraction of multilayer graphene GP550.
Example 7
A heat-dissipating coating was prepared according to the method of example 3, except that few graphene layers in the raw material were replaced with the same mass fraction of multilayer graphene GP550.
Example 8
A heat-dissipating coating was prepared according to the method of example 4, except that few graphene layers in the raw material were replaced with the same mass fraction of multilayer graphene GP550.
Example 9
A heat-dissipating coating was prepared in the same manner as in example 4 except that the amount of the dispersant added to the raw material was 5 parts.
Example 10
A heat-dissipating coating was prepared in the same manner as in example 4 except that the amount of dispersant added to the raw material was 1 part.
Example 11
A heat-dissipating coating was prepared in the same manner as in example 4 except that the thixotropic agent was added to the raw material in an amount of 5 parts.
Example 12
A heat dissipating coating was prepared as in example 4, except that no thixotropic agent was added to the raw materials.
Example 13
A heat-dissipating coating was prepared in the same manner as in example 4 except that the leveling agent was added to the raw material in an amount of 2 parts.
Example 14
A heat-dissipating coating was prepared as in example 4, except that no leveling agent was added to the raw materials.
Comparative example 1
A heat-dissipating coating was prepared according to the method of example 4, except that the few-layer graphene in the raw material was replaced with spherical alumina of the same mass fraction.
Comparative example 2
A heat-dissipating coating was prepared according to the method of example 4, except that the few-layer graphene in the raw material was replaced with spherical zinc oxide of the same mass fraction.
Comparative example 3
A heat dissipating coating was prepared as in example 4, except that the raw material replaced the ceramic resin with an equal mass fraction of epoxy resin.
Comparative example 4
A heat-dissipating coating was prepared as in example 4, except that no dispersant was added to the raw materials.
Comparative example 5
A heat-dissipating coating was prepared as in example 4, except that the ceramic resin in the raw material was replaced with a potassium silicate inorganic resin.
Comparative example 6
A heat-dissipating coating was prepared as in example 4, except that the raw materials included:
comparative example 7
A heat-dissipating coating was prepared as in example 4, except that the raw materials included:
test case
The viscosity of the heat-dissipating paint of the above examples and comparative examples was measured by a six-speed rotational viscometer of an epoxy resin system at 25℃using GB/T22235-2008 "measurement and detection Standard for liquid viscosity", and the results of the measurements are shown in Table 1.
The heat dissipation coating prepared by adopting the examples and the comparative examples is sprayed on a fin type electric heating pipe, is kept stand for 20min at the room temperature of 25 ℃ after being sprayed, and is baked for 30min at the temperature of 200 ℃ to form the fin type electric heating pipe with a heat dissipation layer, wherein the thickness of the heat dissipation layer is 25 mu m.
The heat dissipation coating prepared by adopting the examples and the comparative examples is sprayed on a material plate with the thickness of 25 μm, wherein the material plate is 10cm multiplied by 10cm and has the same surface material as the fin type electric heating pipe, the heat dissipation coating is kept stand for 20min at the room temperature of 25 ℃ after being sprayed, and then is baked for 30min at the temperature of 200 ℃ to form a substrate with a heat dissipation layer.
Performance testing of a heat spreader layer, comprising:
conventional adhesion test: substrates with heat dissipation layers were tested using the hundred method using ASTM D3359 "test standard for adhesion with tape", using american 3M brand 610 paint adhesion test tape, the test results are shown in table 1.
Quick cooling adhesion test: the substrate with the heat dissipation layer was heated to 400 ℃ with a muffle furnace, cooled in cold water with a standing horse, taken out of the water, tested for adhesion according to the hundred-gram method, and the test results are shown in table 1.
Pencil hardness test: the substrate with the heat dissipation layer is coated with GB/T6739-2006 color paint and varnish: paint film hardness detection standard is measured by a pencil method, a Ai Ruipu QHQ-A hand-push pencil hardness tester paint film scratch hardness tester three-in-one paint hardness tester is used, and the test results are shown in table 1.
Impact resistance test: the substrate with the heat dissipation layer was tested using GB/T1732-1993 paint film impact test Standard, laiyte instruments and equipment limited QCJ paint film impact tester paint film impactor, and the test results are shown in Table 1.
Salt spray resistance test: GB/T1771-2007 Standard for measuring neutral salt spray resistance of paint and varnish was used for a substrate having a Heat-dissipating layer, and a salt spray tank of the American Q-LAB brand Q-FOG SSP was used, and the test results are shown in Table 1.
Fin type electric heating tube thermal test: at an initial room temperature of 20℃and an area of 50m 2 The fin type electric heating tube with the heat dissipation layer is placed in the middle of a room with the height of 3mThe surface load of the electric heating tube is 3W/cm 2 An effective heating area of 225cm 2 After the electric heating, the surface temperature was measured using a U.S. Phillips FLIR E95 (measuring range-20-1500 ℃, measuring accuracy.+ -. 2%) high-accuracy hand-held infrared thermal imager industrial thermometer, wherein the surface temperature of the fin type electric heating tube without the heat dissipation layer was 500 ℃, and the room temperature was recorded every 5 minutes, and the time when the room temperature reached 35 ℃ was measured, and the test results are shown in Table 2.
The test results are shown in Table 2.
TABLE 1
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Wherein, taking "> 3000h" as an example, the salt spray resistance duration is longer than 3000h; the salt spray resistance duration is less than 2000h represented by '2000 h <', and other expression modes are similar.
TABLE 2
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As can be seen from tables 1 and 2:
(1) Example 4 compared with examples 9-10, it can be seen that if less dispersant is added, the slurry has poor wettability to the powder after the powder is added, and there is a possibility that the production time is long; if the dispersant is added more, the cost is high, the organic matter storage is more, and the problems of great smoke and smell can be caused when the temperature is heated to more than 200 ℃.
(2) Compared with examples 11-12, it can be seen that if the thixotropic agent is not added, sagging is easy in the spraying construction process, the spraying construction efficiency is affected, for example, the spraying technology is not good, the sprayed objects are easy to discard, if the thixotropic agent is too much added, the paint film surface may be uneven and has orange peel, the appearance is affected, the spraying technology is not good, the bottom leakage is easy to occur, and the salt spray resistance is reduced.
(3) Example 4 compared with examples 13-14, it can be seen that if no leveling agent is added, the paint film may have uneven surface, and the appearance is affected, the leveling agent is excessively added, the paint film surface may have more bubble points, and many bubble points exist in the paint film after drying and curing, which has an effect on the protection, rust is generated in a humid environment for a long time, and the paint film falls off over time.
(4) Compared with example 4 and example 8, it can be seen that the example with less graphene layer has a better heat dissipation effect than the multilayer graphene layer, because the graphene layer has anisotropy in the structure of the layered graphene layer, has excellent electric and thermal conductivity in the parallel direction of the layered graphene layer, and has lower electric and thermal conductivity in the direction perpendicular to the layered graphene layer than in the parallel direction.
(5) Example 4 compared to comparative examples 1-2, it can be seen that the graphene material has better heat dissipation than spherical alumina, zinc oxide.
(6) In the embodiment 4, compared with the embodiments 1-3 and the embodiments 5-7, the oxidation temperature of the graphene is 400 ℃, the temperatures of the embodiments 1-3 and the embodiments 5-7 are higher than 400 ℃, the graphene is oxidized during long-time use, the heat dissipation effect is affected, in the test that the current is continuously conducted for 6 months under the condition that the air conditioner is not opened in spring, summer and autumn three seasons (4 months-10 months), the room temperature of the 10 month end test is the same as the room temperature of the 4 month start test, the surface heating temperature rise is not more than 2%, and the agreed requirement can be met.
(7) Example 4 in comparison with comparative examples 3 to 5, comparative example 4 was cured at 150℃for 30 minutes after the film formation was changed to epoxy resin, and the paint film was smoky and odorous when the temperature reached 200℃or higher after the energization. After the continuous power-on heating is carried out for 1 hour, the paint film is atomized and falls off. In the production process of comparative example 4, powder is always held and is not easy to uniformly disperse in the coating, the rotating speed of a dispersing machine is increased, and the production time is prolonged. Example 5 potassium silicate is a film former, has poor wettability to powder, has poor film forming property when sprayed on a substrate, and requires high spraying skill. After the film is solidified, the adhesive force is poor and is only 3-4B, the paint film is porous, moisture easily enters the coating to reach the interface between the coating and the substrate, the substrate is rusted, and the paint film can fall off for a long time. Therefore, the high-temperature-resistant (used below 400 ℃) heat dissipation coating prepared by matching the ceramic resin with graphene has film forming property and high temperature resistance, has good adhesive force to metal and ceramic, can not deteriorate even if the ceramic resin is put into cold water for cooling under the high-temperature condition, has the characteristics of convenience in use, long storage period, good stability and the like, and the comparative example 5 adopts silicate inorganic resin, so that the formed coating has a porous structure and poor heat dissipation effect.
(10) As can be seen from comparative examples 6-7, comparative example 6 is a powder with reduced amounts of film former providing film forming and adhesion properties and with increased amounts of powder providing water blocking and shrink resistance. Comparative example 6 had too little film former, resulting in a film with poor adhesion to the substrate of only 3B. Comparative example 7 is to increase the amount of film former and decrease the amount of powder, and the shrinkage stress during the curing process of the paint film is too strong, resulting in cracking of the paint film. Neither embodiment can be sold as a commodity.
From the above examples and comparative examples, it can be seen that:
1. according to the application, the inorganic ceramic resin is used as a high-temperature resistant film forming material, and is matched with the high thermal conductivity and high thermal radiation conversion rate of graphene, and auxiliary substance stable coatings such as a dispersing agent, a filler and the like, so that the high-temperature resistant film forming material can be applied to the field of high-temperature heat dissipation.
2. The heat-dissipating paint has good adhesive force to metal and ceramic, and meanwhile, the heat-dissipating paint is instantly put into cold water for cooling under the high temperature condition, so that the adhesive force is not deteriorated, and the test is performed in the hundred-grid test 5B. Solves the difficulty that the adhesive force is reduced due to the abrupt temperature change caused by careless water drop on the fin type electric heating tube which generates heat in use.
3. The heat dissipation coating can be stored for more than 6 months at a shade place at 25 ℃ and has long storage life.
4. The heat dissipation coating is simple and convenient to construct. For example, when the adhesive is used for a fin type electric heating pipe, the adhesive can be cured after being placed for 15-20 minutes at normal temperature and baked for half an hour at 200-260 ℃, and excellent adhesion is generated, so that the surface temperature of the fin type electric heating pipe when the electric heating pipe is electrified and heated is reduced.
5. The heat-dissipating coating can adjust viscosity, thixotropy and fluidity according to different construction processes by adjusting the proportion of the main agent and the solvent, and has wide applicability.
6. The heat-dissipating paint of the application has incombustibility, is stable at 600 ℃ and generates most of SiO which can not burn at more than 800 DEG C 2 The safety is higher than that of polyurethane resin, polyester resin and epoxy resin as film forming materials.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the application, which are described in detail and are not to be construed as limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
Claims (10)
1. The heat dissipation coating is characterized by comprising 40-60 parts by weight of ceramic resin, based on 100 parts by weight of the total heat dissipation coating, of graphene, a dispersing agent, a filler and a solvent.
2. The heat-dissipating coating of claim 1, wherein the heat-dissipating coating satisfies at least one of the following conditions, based on 100 parts by total mass of the heat-dissipating coating:
(1) The mass portion of the graphene is 3-12;
(2) The mass part of the dispersing agent is 1-2;
(3) The mass portion of the filler is 20-30;
(4) The mass portion of the solvent is 10-20.
3. The heat dissipating coating of claim 1, wherein said ceramic resin comprises an oxide sol-based ceramic resin;
optionally, the oxide sol-type ceramic resin includes at least one of a silica sol, an alumina sol, a colloidal zirconia sol, a ceria sol, and a nickel oxide sol.
4. The heat dissipating coating of claim 1, wherein the graphene satisfies at least one of the following conditions:
(1) The number of layers of the graphene is 1-20;
(2) The particle size D50 of the graphene is smaller than 6 mu m;
(3) The graphene includes at least one of graphene oxide, reduced graphene oxide, and doped graphene.
5. The heat-dissipating coating of claim 1, wherein the heat-dissipating coating satisfies at least one of the following conditions:
(1) The dispersing agent comprises at least one of ammonium carboxylate salt, polyester phosphate ester and polycaprolactone polyurethane; optionally, the molecular weight of the dispersing agent is 2000-3000;
(2) The filler comprises at least one of mica powder and talcum powder; optionally, the diameter of the filler is 400-600 meshes.
6. The heat-dissipating coating of any of claims 1-5, wherein the heat-dissipating coating further comprises an auxiliary agent; optionally, the auxiliary agent comprises at least one of a coupling agent, an acidity regulator, a thixotropic agent and a leveling agent.
7. The heat dissipating coating of claim 6, wherein said auxiliary agent satisfies at least one of the following conditions:
(1) The coupling agent comprises a silane coupling agent; optionally, the coupling agent is 2-5 parts by mass;
(2) The acidity regulator comprises at least one of acetic acid and lactic acid; optionally, the acid regulator is 0.1 to 1 part based on 100 parts of the total mass of the heat dissipation coating;
(3) The thixotropic agent comprises fumed silica; optionally, 1-3 parts of thixotropic agent based on 100 parts of the total mass of the heat dissipation coating;
(4) The leveling agent comprises an organosilicon leveling agent; optionally, the leveling agent is 0.1 to 1 part based on 100 parts of the total mass of the heat dissipation coating.
8. A method of preparing the heat-dissipating coating of any one of claims 1-7, comprising:
and mixing ceramic resin, graphene, a dispersing agent, a filler and a solvent to prepare the heat dissipation coating.
9. The method of manufacturing of claim 8, wherein the heat dissipating coating further comprises an auxiliary agent, optionally comprising at least one of a coupling agent, an acidity regulator, a thixotropic agent, and a leveling agent, the method of manufacturing comprising:
mixing ceramic resin, a coupling agent, an acid regulator, a dispersing agent, a leveling agent and a solvent, and then adding a filler, a thixotropic agent and graphene for mixing to prepare the heat dissipation coating.
10. A heat generating device comprising a heat dissipation layer formed from the heat dissipation coating of any one of claims 1-7.
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