A method of preparing a graphene glass powder aqueous coating and a method of using the same

Abstract

This invention relates to the field of high-temperature resistant water-based coatings, specifically to a method for preparing and using a high-thermal-conductivity, high-temperature resistant graphene glass powder water-based coating. The method involves adding graphene oxide with a carbon-to-oxygen ratio of 1.1-1.5:1 and a reducing agent to a water-soluble resin premix of glass powder. After uniform mixing, a high-thermal-conductivity, high-temperature resistant graphene glass powder water-based coating is obtained. The water-soluble resin premix comprises uniformly mixed glass powder with a melting point of 200-500℃, a water-soluble resin binder, a dispersant, and water. The prepared water-based coating is uniformly sprayed onto the surface of the substrate. Then, it undergoes segmented heating and baking for curing. After cooling, a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating is obtained. In the water-based coating provided by this invention, graphene is fully dispersed in the coating and self-assembles to form a thermally conductive network during the baking and curing process, thereby improving the thermal conductivity of the coating.

Description

Technical Field

[0001] This invention relates to the field of water-based thermally conductive coatings, and particularly to a method for preparing and using a graphene glass powder water-based coating. Background Technology

[0002] Existing high-temperature resistant coatings often require the addition of a certain amount of low-melting-point glass powder to enhance the coating's hardness, increase adhesion, and improve its crack resistance. In sintered coating systems, low-melting-point glass powder forms the main paint film, provides overall adhesion, and enhances the material's wear and heat resistance. Although it exhibits good high-temperature resistance, the low thermal conductivity of glass powder means the coating's thermal conductivity still needs improvement. Graphene is a material with excellent thermal conductivity. Existing technologies, such as the Chinese invention patent (CN111073503A) titled "A High-Temperature Resistant, High-Emissivity Anticorrosive Coating," incorporate graphene into low-melting-point glass powder to improve the coating's heat dissipation. While this method can improve heat dissipation to some extent, it also has drawbacks. Graphene is difficult to disperse in aqueous systems, and direct addition can easily lead to agglomeration of the thermally conductive material, limiting the graphene's performance. Furthermore, graphene has poor adhesion; excessive addition can actually hinder film formation. In addition, small-diameter graphene cannot form a network in coating systems. Only large-diameter graphene can improve thermal conductivity. However, the preparation of large-diameter graphene is difficult and costly. These problems limit the widespread application of high-temperature resistant thermally conductive coatings. Summary of the Invention

[0003] To overcome the shortcomings of existing technologies, this invention prepares a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder aqueous coating, using graphene oxide as the main filler, hydrazine hydrate, vitamin C, glucose, and other reagents as reducing agents, along with glass powder, other coating additives, and water. During the sintering process, the graphene oxide is self-assembled to form a high-thermal-conductivity reduced graphene oxide pathway, and the glass powder is sintered to form a solidified coating, thus solving the problem of the difficulty in dispersing and applying reduced graphene oxide in solvent systems.

[0004] The first objective of this invention is to provide a high thermal conductivity, high-temperature resistant graphene glass powder water-based coating. During the curing and baking process, graphene oxide self-assembles into a high thermal conductivity network, exhibiting high hardness, high temperature resistance, and high adhesion after curing, thus possessing high thermal conductivity. The technical solution adopted by this invention to solve its technical problem is as follows:

[0005] The following ingredients are included, measured in parts by weight:

[0006] Glass powder: 50-100 parts

[0007] Graphene oxide aqueous slurry: 96-195 parts

[0008] Water-soluble resin adhesive: 8-16 parts

[0009] Dispersant: 1.6-3.2 parts

[0010] Water: 32-64 parts

[0011] Reducing agent: 0.8-1.6 parts

[0012] The glass powder has a melting point of 200-500℃; the graphene oxide is prepared by the modified Hummers method with a carbon-to-oxygen ratio of 1.1-1.5:1 and a sheet size of 3-40μm.

[0013] In a further technical solution, the glass powder with a melting point of 200-500℃ comprises, by weight, the following raw materials.

[0014] Silica glass powder: 50-100 parts

[0015] Titanium dioxide glass powder; 0-50 parts

[0016] Alumina glass powder; 0-35 parts

[0017] Bismuthate glass powder: 0-15 parts

[0018] Silica boron metal salt glass powder: 0-15 parts.

[0019] In a further technical solution, the graphene oxide aqueous slurry, in parts by weight, comprises the following raw materials.

[0020] Graphene oxide: 1.2-19.6 parts

[0021] Water: 94.8-175.4 parts.

[0022] In a further technical solution, the water-soluble resin adhesive is one or more of the following: water-based polyurethane resin, water-based acrylic resin, water-based alkyd resin, water-based polyester resin, and water-based epoxy resin.

[0023] In a further technical solution, the water-soluble resin adhesive is one or more of the following: water-based polyurethane resin, water-based acrylic resin, water-based alkyd resin, water-based polyester resin, and water-based epoxy resin, all with a decomposition temperature of 100-200℃.

[0024] In a further technical solution, the dispersant is one or more of the following: octadeceneamine acetate, alkyl quaternary ammonium salt, aminopropylamine dioleate, quaternary ammonium salt, and polyaminoamide phosphate.

[0025] In a further technical solution, the reducing agent is one or more of hydrazine hydrate, vitamin C, and glucose.

[0026] The second objective of this invention is to provide a method for preparing a high thermal conductivity, high-temperature resistant graphene glass powder water-based coating, comprising the following steps:

[0027] S1: Preparation of graphene oxide slurry

[0028] By weight, 1.2-19.6 parts of graphene oxide are mixed with 94.8-175.4 parts of water, and the mixture is stirred at 500 r / min for 0.5 h at 50 °C. The mixture is then cooled to room temperature for later use.

[0029] S2: Preparation of water-soluble resin premix of glass powder

[0030] According to the above-mentioned weight proportions, the glass powder with a melting point of 200-500℃ is compounded, and the powder is melted at a high temperature of 400-600℃ in air to form an amorphous eutectic. This eutectic is then ground and pulverized into glass powder with a particle size of 5-10μm and a melting point of 200-500℃. According to the above-mentioned weight proportions, the water-soluble resin binder, water, and dispersant are dispersed and mixed at 500 r / min at room temperature for 0.5 h. The fully mixed glass powder with a melting point of 200-500℃ is then added, and the mixture is mixed at 1000 r / min at 50℃ for 1-2 h. The mixture is then cooled to room temperature to obtain a glass powder water-soluble resin premix.

[0031] S3: Preparation of high-temperature resistant, high-thermal-conductivity graphene glass powder water-based coatings

[0032] According to the above-mentioned weight proportions, the graphene oxide slurry and reducing agent are mixed at 1200 r / min at 50°C for 0.5 h for weak reduction, and then the glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating.

[0033] The third objective of this invention is to provide a method for applying a high-temperature, high-thermal-conductivity water-based coating of graphene oxide glass powder.

[0034] A substrate with a temperature resistance of over 200℃ is selected. After sanding to remove surface rust and stains, rinsing with deionized water and drying, the prepared water-based coating is evenly sprayed onto the substrate surface. Then, it is baked and cured. During the curing process, the temperature is increased from room temperature to 100℃ at a rate of 10℃ / min and held for 10 minutes; then increased to 200℃ at a rate of 10℃ / min and held for 10 minutes; finally, the temperature is increased to 300-500℃ at a rate of 10℃ / min and held for 20 minutes. After cooling, a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating is obtained. During the heating process, the graphene oxide is simultaneously thermally reduced, causing the graphene oxide to self-assemble and form a thermally conductive network, thereby improving the coating's thermal conductivity.

[0035] The beneficial effects of this invention are:

[0036] The high thermal conductivity graphene oxide glass powder waterborne coating prepared in this application utilizes the excellent dispersibility in water exhibited by the numerous oxygen-containing groups such as carbonyl, carboxyl, hydroxyl, and epoxy groups on the surface of graphene oxide, effectively solving the problem of the extreme difficulty in dispersing reduced graphene oxide in waterborne coating systems. By using a reducing agent during the coating preparation process, the graphene oxide undergoes preliminary weak reduction in the coating system. During the subsequent baking and curing process, the self-assembly effect of the graphene oxide reduction process forms a highly thermally conductive reduced graphene oxide network, thereby achieving the purpose of improving the thermal conductivity of the coating.

[0037] This invention utilizes the surface defects present during the reduction and self-assembly of graphene oxide. High-temperature resistant glass powder is embedded into these defects and the surface. After high-temperature melting, the glass powder forms a dense, highly adhesive bonding system, solving the problem that reduced graphene oxide is difficult to adhere to the application surface in practical applications. Detailed Implementation

[0038] The present invention will be further described below with reference to specific embodiments, but these should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art. Unless otherwise specified, the reagents, methods, and equipment used in the present invention are conventional reagents, methods, and equipment in this technical field, and there are no specific restrictions on their sources; they can be purchased from the market or prepared according to conventional methods well known to those skilled in the art.

[0039] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.

[0040] The technical solution of the present invention is illustrated below through specific embodiments. It should be understood that the one or more steps mentioned in the present invention do not preclude the existence of other methods and steps before or after the combined steps, or that other methods and steps may be inserted between these explicitly mentioned steps. It should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Unless otherwise stated, the numbering of each method step is only for the purpose of identifying each method step, and not for limiting the order of each method or limiting the scope of the present invention. Changes or adjustments to their relative relationships, without substantial changes to the technical content, can also be considered as within the scope of the present invention.

[0041] The foregoing description of specific exemplary embodiments of the invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it will be apparent that many changes and variations can be made in accordance with the foregoing teachings. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various different exemplary embodiments of the invention, as well as various different choices and variations. The scope of the invention is intended to be defined by the claims and their equivalents.

[0042] Example 1

[0043] A high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating, comprising the following raw materials in parts by weight:

[0044] Glass powder with a melting point of 300℃: 76 parts

[0045] 5wt% graphene oxide aqueous slurry: 152 parts

[0046] Water-based acrylic resin: 12.7 parts

[0047] Octadecyleneamine acetate: 2.4 parts

[0048] Water: 50.6 parts

[0049] Vitamin C: 0.8 parts

[0050] Among them: glass powder with a melting point of 300℃, expressed in parts by weight, includes the following raw materials:

[0051] Silica glass powder: 50 parts

[0052] Titanium dioxide glass powder: 12 parts

[0053] Alumina glass powder: 1 part

[0054] Bismuthate glass powder: 1 part

[0055] 12 parts of silica boron metal salt glass powder

[0056] The preparation of the above-mentioned high-temperature resistant and high-thermal-conductivity water-based coating of graphene oxide glass powder includes the following steps:

[0057] S1: Preparation of graphene oxide slurry

[0058] Graphene oxide with a solid content of 5 wt%, a sheet size of 40 μm, and a carbon-to-oxygen ratio of 1.5:1 was prepared according to the modified Hummers method and cooled to room temperature for later use.

[0059] S2: Preparation of water-soluble resin premix of glass powder

[0060] According to the above-mentioned weight proportions, the glass powder with a melting point of 300℃ is compounded, and the powder is melted at 400℃ in air to form an amorphous eutectic. After grinding and pulverizing, glass powder with a melting point of 300℃ and a particle size of 5μm is obtained. According to the above-mentioned weight proportions, waterborne acrylic resin, water, and octadeceneamine acetate are dispersed and mixed at 500r / min at room temperature for 0.5h. The fully mixed glass powder with a melting point of 300℃ is added, and the mixture is mixed at 1000r / min at 50℃ for 1-2h. After cooling to room temperature, a water-soluble resin premix of glass powder is obtained.

[0061] S3: Preparation of high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coatings

[0062] According to the above-mentioned weight proportions, the graphene oxide slurry and vitamin C are mixed at 1200 r / min at 50°C for 0.5 h with weak reduction, and then the glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating.

[0063] Example 2

[0064] Compared with Example 1, the difference in this example is that 76 parts of glass powder with a melting point of 300°C are replaced with 76 parts of glass powder with a melting point of 500°C.

[0065] A high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating, comprising the following raw materials in parts by weight:

[0066] Glass powder with a melting point of 500℃: 76 parts

[0067] 5wt% graphene oxide aqueous slurry: 152 parts

[0068] Water-based acrylic resin: 12.7 parts

[0069] Octadecyleneamine acetate: 2.4 parts

[0070] Water: 50.6 parts

[0071] Vitamin C: 0.8 parts

[0072] Among them: glass powder with a melting point of 500℃, in parts by weight, includes the following raw materials:

[0073] Silica glass powder: 60 parts

[0074] Titanium dioxide glass powder: 8 parts

[0075] Alumina glass powder: 9 parts

[0076] Bismuthate glass powder: 5 parts

[0077] 4 parts of silica boron metal salt glass powder

[0078] The preparation of the above-mentioned high-temperature resistant and high-thermal-conductivity water-based coating of graphene oxide glass powder includes the following steps:

[0079] S1: Preparation of graphene oxide slurry

[0080] Graphene oxide with a solid content of 5 wt%, a sheet size of 40 μm, and a carbon-to-oxygen ratio of 1.5:1 was prepared according to the modified Hummers method and cooled to room temperature for later use.

[0081] S2: Preparation of water-soluble resin premix of glass powder

[0082] According to the above-mentioned weight proportions, the glass powder with a melting point of 500℃ is compounded, and the powder is melted at 600℃ in air to form an amorphous eutectic. After grinding and pulverizing, glass powder with a melting point of 500℃ and a particle size of 5μm is obtained. According to the above-mentioned weight proportions, waterborne acrylic resin, water, and octadeceneamine acetate are dispersed and mixed at 500r / min at room temperature for 0.5h. The fully mixed glass powder with a melting point of 500℃ is added, and the mixture is mixed at 1000r / min at 50℃ for 1-2h. After cooling to room temperature, a water-soluble resin premix of glass powder is obtained.

[0083] S3: Preparation of high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coatings

[0084] According to the above-mentioned weight proportions, the graphene oxide slurry and vitamin C are mixed at 1200 r / min at 50°C for 0.5 h with weak reduction, and then the glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating.

[0085] Example 3

[0086] Compared with Example 1, the difference in this example is that the reducing agent vitamin C is replaced with hydrazine hydrate.

[0087] A high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating, comprising the following raw materials in parts by weight:

[0088] Glass powder with a melting point of 300℃: 76 parts

[0089] 5wt% graphene oxide aqueous slurry: 152 parts

[0090] Water-based acrylic resin: 12.7 parts

[0091] Octadecyleneamine acetate: 2.4 parts

[0092] Water: 50.6 parts

[0093] Hydrazine hydrate: 0.8 parts

[0094] Among them: glass powder with a melting point of 300℃, expressed in parts by weight, includes the following raw materials:

[0095] Silica glass powder: 50 parts

[0096] Titanium dioxide glass powder: 12 parts

[0097] Alumina glass powder: 1 part

[0098] Bismuthate glass powder: 1 part

[0099] 12 parts of silica boron metal salt glass powder

[0100] The preparation of the above-mentioned high-temperature resistant and high-thermal-conductivity water-based coating of graphene oxide glass powder includes the following steps:

[0101] S1: Preparation of graphene oxide slurry

[0102] Graphene oxide with a solid content of 5 wt%, a sheet size of 40 μm, and a carbon-to-oxygen ratio of 1.5:1 was prepared according to the modified Hummers method and cooled to room temperature for later use.

[0103] S2: Preparation of water-soluble resin premix of glass powder

[0104] According to the above-mentioned weight proportions, the glass powder with a melting point of 300℃ is compounded, and the powder is melted at 400℃ in air to form an amorphous eutectic. After grinding and pulverizing, glass powder with a melting point of 300℃ and a particle size of 5μm is obtained. According to the above-mentioned weight proportions, waterborne acrylic resin, water, and octadeceneamine acetate are dispersed and mixed at 500r / min at room temperature for 0.5h. The fully mixed glass powder with a melting point of 300℃ is added, and the mixture is mixed at 1000r / min at 50℃ for 1-2h. After cooling to room temperature, a water-soluble resin premix of glass powder is obtained.

[0105] S3: Preparation of high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coatings

[0106] According to the above-mentioned weight proportions, the graphene oxide slurry and hydrazine hydrate are mixed and weakly reduced at 1200 r / min and 50°C for 0.5 h. The glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant and high thermal conductivity graphene oxide glass powder water-based coating.

[0107] Example 4

[0108] Compared with Example 1, the difference in this example is that the solid content of graphene oxide is 5wt%, the carbon-oxygen ratio is 1.2:1, and the sheet size is 40um.

[0109] A high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating, comprising the following raw materials in parts by weight:

[0110] Glass powder with a melting point of 300℃: 76 parts

[0111] 5wt% graphene oxide aqueous slurry: 152 parts

[0112] Water-based acrylic resin: 12.7 parts

[0113] Octadecyleneamine acetate: 2.4 parts

[0114] Water: 50.6 parts

[0115] Vitamin C: 0.8 parts

[0116] Among them: glass powder with a melting point of 300℃, expressed in parts by weight, includes the following raw materials:

[0117] Silica glass powder: 50 parts

[0118] Titanium dioxide glass powder: 12 parts

[0119] Alumina glass powder: 1 part

[0120] Bismuthate glass powder: 1 part

[0121] 12 parts of silica boron metal salt glass powder

[0122] The preparation of the above-mentioned high-temperature resistant and high-thermal-conductivity water-based coating of graphene oxide glass powder includes the following steps:

[0123] S1: Preparation of graphene oxide slurry

[0124] Graphene oxide with a solid content of 5 wt%, a sheet size of 40 μm, and a carbon-to-oxygen ratio of 1.2:1 was prepared according to the modified Hummers method and cooled to room temperature for later use.

[0125] S2: Preparation of water-soluble resin premix of glass powder

[0126] According to the above-mentioned weight proportions, the glass powder with a melting point of 300℃ is compounded, and the powder is melted at 400℃ in air to form an amorphous eutectic. After grinding and pulverizing, glass powder with a melting point of 300℃ and a particle size of 5μm is obtained. According to the above-mentioned weight proportions, waterborne acrylic resin, water, and octadeceneamine acetate are dispersed and mixed at 500r / min at room temperature for 0.5h. The fully mixed glass powder with a melting point of 300℃ is added, and the mixture is mixed at 1000r / min at 50℃ for 1-2h. After cooling to room temperature, a water-soluble resin premix of glass powder is obtained.

[0127] S3: Preparation of high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coatings

[0128] According to the above-mentioned weight proportions, the graphene oxide slurry and vitamin C are mixed at 1200 r / min at 50°C for 0.5 h with weak reduction, and then the glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating.

[0129] Example 5

[0130] Compared with Example 1, the difference in this example is that the solid content of graphene oxide is 8wt%, the carbon-oxygen ratio is 1.5:1, and the sheet size is 40um.

[0131] A high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating, comprising the following raw materials in parts by weight:

[0132] Glass powder with a melting point of 300℃: 76 parts

[0133] 8wt% graphene oxide aqueous slurry: 152 parts

[0134] Water-based acrylic resin: 12.7 parts

[0135] Octadecyleneamine acetate: 2.4 parts

[0136] Water: 50.6 parts

[0137] Vitamin C: 0.8 parts

[0138] Among them: glass powder with a melting point of 300℃, expressed in parts by weight, includes the following raw materials:

[0139] Silica glass powder: 50 parts

[0140] Titanium dioxide glass powder: 12 parts

[0141] Alumina glass powder: 1 part

[0142] Bismuthate glass powder: 1 part

[0143] 12 parts of silica boron metal salt glass powder

[0144] The preparation of the above-mentioned high-temperature resistant and high-thermal-conductivity water-based coating of graphene oxide glass powder includes the following steps:

[0145] S1: Preparation of graphene oxide slurry

[0146] Graphene oxide with a solid content of 8 wt%, a sheet size of 40 μm, and a carbon-to-oxygen ratio of 1.5:1 was prepared according to the modified Hummers method and cooled to room temperature for later use.

[0147] S2: Preparation of water-soluble resin premix of glass powder

[0148] According to the above-mentioned weight proportions, the glass powder with a melting point of 300℃ is compounded, and the powder is melted at 400℃ in air to form an amorphous eutectic. After grinding and pulverizing, glass powder with a melting point of 300℃ and a particle size of 5μm is obtained. According to the above-mentioned weight proportions, waterborne acrylic resin, water, and octadeceneamine acetate are dispersed and mixed at 500r / min at room temperature for 0.5h. The fully mixed glass powder with a melting point of 300℃ is added, and the mixture is mixed at 1000r / min at 50℃ for 1-2h. After cooling to room temperature, a water-soluble resin premix of glass powder is obtained.

[0149] S3: Preparation of high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coatings

[0150] According to the above-mentioned weight proportions, the graphene oxide slurry and vitamin C are mixed at 1200 r / min at 50°C for 0.5 h with weak reduction, and then the glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating.

[0151] Example 6

[0152] Compared with Example 1, the difference in this example is that the 152 parts of 5wt% graphene oxide aqueous slurry in Example 1 are replaced with 5wt% graphene slurry with a sheet diameter of 40μm.

[0153] A high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coating, comprising the following raw materials in parts by weight:

[0154] Glass powder with a melting point of 300℃: 76 parts

[0155] 5wt% graphite ink slurry: 152 parts

[0156] Water-based acrylic resin: 12.7 parts

[0157] Octadecyleneamine acetate: 2.4 parts

[0158] Water: 50.6 parts

[0159] Vitamin C: 0.8 parts

[0160] Among them: glass powder with a melting point of 300℃, expressed in parts by weight, includes the following raw materials:

[0161] Silica glass powder: 50 parts

[0162] Titanium dioxide glass powder: 12 parts

[0163] Alumina glass powder: 1 part

[0164] Bismuthate glass powder: 1 part

[0165] 12 parts of silica boron metal salt glass powder

[0166] The preparation of the above-mentioned high-temperature resistant and high-thermal-conductivity water-based coating of graphene oxide glass powder includes the following steps:

[0167] S1: Preparation of graphene oxide slurry

[0168] Prepare the corresponding raw materials, add each raw material at room temperature, mix at 500 r / min for 0.5 h to obtain a graphite slurry with a solid content of 5 wt% and a flake size of 40 μm, and let it stand at room temperature for later use.

[0169] S2: Preparation of water-soluble resin premix of glass powder

[0170] According to the above-mentioned weight proportions, the glass powder with a melting point of 300℃ is compounded, and the powder is melted at 400℃ in air to form an amorphous eutectic. After grinding and pulverizing, glass powder with a melting point of 300℃ and a particle size of 5μm is obtained. According to the above-mentioned weight proportions, waterborne acrylic resin, water, and octadeceneamine acetate are dispersed and mixed at 500r / min at room temperature for 0.5h. The fully mixed glass powder with a melting point of 300℃ is added, and the mixture is mixed at 1000r / min at 50℃ for 1-2h. After cooling to room temperature, a water-soluble resin premix of glass powder is obtained.

[0171] S3: Preparation of high-temperature resistant, high-thermal-conductivity water-based coatings using graphite glass powder

[0172] According to the above-mentioned weight proportions, the graphite slurry and vitamin C are mixed at 1200 r / min at 50°C for 0.5 h, and the glass powder water-soluble resin premix of the above-mentioned weight proportions is added and mixed at 1200 r / min and cooled to room temperature to obtain a high-temperature resistant, high thermal conductivity graphene oxide glass powder water-based coating.

[0173] Example 7

[0174] Compared with Example 1, the difference in this example is that the 152 parts of 5wt% graphene oxide slurry in Example 1 are replaced with an equal part of reduced graphene oxide, that is, 7.6 parts of reduced graphene oxide with a sheet diameter of 40μm.

[0175] Example 8

[0176] The coating prepared in Example 1 was sprayed and then baked and cured.

[0177] Prepare a copper substrate with dimensions of 0.05*100*100mm. Remove surface rust and stains by sanding with sandpaper. After rinsing with deionized water and drying, spray the water-based coating obtained in Example 1 onto one side of the 100*100mm substrate. Then, bake and cure the coating. During the curing process, the temperature is increased from room temperature to 100℃ at a rate of 10℃ / min and held for 10min. Then, the temperature is increased from 100℃ to 200℃ at a rate of 10℃ / min and held for 20min. Finally, the temperature is increased to 300℃ at a rate of 10℃ / min and held for 20min. After cooling, a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coated copper sheet is obtained.

[0178] The composite copper sheet with a high thermal conductivity graphene oxide glass powder aqueous coating was immersed in a mixed solution of FeCl3 and HCl with a total concentration of 4 mol / L and a molar ratio of 1:3. After 5 minutes, it was removed to obtain a high-temperature resistant, high thermal conductivity graphene oxide glass powder aqueous coating.

[0179] Example 9

[0180] The coating prepared in Example 2 was sprayed and then baked and cured.

[0181] Compared to Example 8, the difference in this example is that the temperature gradient during the curing process is as follows: the temperature is increased from room temperature to 100°C at a rate of 10°C / min and held for 10 minutes; then the temperature is increased from 100°C to 200°C at a rate of 10°C / min and held for 20 minutes; finally, the temperature is increased to 500°C at a rate of 30°C / min and held for 20 minutes. This results in a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder water-based coated copper sheet.

[0182] After undergoing the same copper etching method as in Example 8, a high-temperature resistant, high-thermal-conductivity graphene oxide glass powder aqueous coating was obtained.

[0183] Example 10

[0184] The coating prepared in Example 3 was sprayed and then baked and cured.

[0185] Example 11

[0186] The coating prepared in Example 4 was sprayed and then baked and cured.

[0187] Example 12

[0188] The coating prepared in Example 5 was sprayed and then baked and cured.

[0189] Example 13

[0190] The coating prepared in Example 6 was sprayed and then baked and cured.

[0191] Example 14

[0192] The coating prepared in Example 7 was sprayed and then baked and cured.

[0193] Temperature resistance and thermal conductivity tests:

[0194] According to GB / T 1735—2009 standard, the samples obtained in Examples 8-14 were subjected to temperature resistance tests. The test method was as follows:

[0195] Three samples from the same embodiment in Examples 8-14 were placed in a high-temperature furnace at a specified temperature (280°C for Examples 8, 10, 11, 12, 13, and 14, and 480°C for Example 9). The distance between each sample and the furnace was no less than 100 mm, and the spacing between the samples was no less than 20 mm. The samples were placed in the center of the furnace whenever possible. At the specified temperature, the samples were placed on a sample holder made of a suitable heat-resistant material or placed with the painted side of the sample facing up on a heat-resistant material plate supported by a support for 24 hours. After the specified time, the samples were removed from the oven or high-temperature furnace and allowed to cool to room temperature.

[0196] Inspect the test panel and compare it with an unheated test panel prepared under the same conditions to see if there is any change in the color of the coating or any other damage to the coating. The test result is considered to be consistent between at least two test panels.

[0197] Thermal conductivity tests were performed on the samples obtained in Examples 8-14 using a HotDisk thermal constant analyzer. The test method was as follows:

[0198] Three samples from the same embodiment in Examples 8-14 were cut into circular slices with a radius of 10 mm. The thin film module of a HotDisk thermal constant analyzer was used for testing, with the substrate as the background material, allowing direct measurement of the coating's thermal conductivity. The average of the three tests was taken as the experimental result.

[0199] The test results are as follows:

[0200] Example Example 8 Example 9 Example 10 Example 11 Example 12 Example 13 Example 14 High temperature resistance / ℃ 280 480 280 280 280 280 280 Longitudinal thermal conductivity / W / (m·K) 6.14 5.90 6.72 4.49 8.28 3.22 1.12 In-plane thermal conductivity / W / (m·K) 83.62 80.33 91.52 63.66 110.51 3.61 2.57

[0201] The test results above show that the high-temperature resistance of the coating is related to the composition of the glass powder. Different coating systems with varying temperature tolerances can be obtained by configuring different glass powders. Regarding thermal conductivity, the coatings obtained after baking in Examples 8-12 generally exhibit an in-plane thermal conductivity of over 60 W / (m·K). This demonstrates that graphene successfully constructs a conductive network within the coating system, providing a certain degree of improvement in thermal conductivity. Furthermore, the longitudinal thermal conductivity is also generally higher than that of typical graphene thermal conductive films. The applicant believes that because the assembly direction of graphene oxide is not necessarily horizontal, there will be a certain angle when forming the thermal conductive network, thus improving the longitudinal thermal conductivity. Example 13, however, uses a direct addition of graphite. Because graphite does not have self-assembling properties, the reduced graphene oxide cannot form a thermal conductive network, resulting in a poor improvement in the coating's thermal conductivity. Similarly, the improvement in thermal conductivity in Example 14 was not ideal. The applicant believes there are two main reasons for this: firstly, the reduced graphene oxide has lost its self-contained properties and cannot form a thermally conductive network; secondly, the reduced graphene oxide is difficult to dissolve in the system, so the amount that can be added is limited, and the improvement in thermal conductivity is not ideal.

[0202] The foregoing description of specific exemplary embodiments of the invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it will be apparent that many changes and variations can be made in accordance with the foregoing teachings. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various different exemplary embodiments of the invention, as well as various different choices and variations. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A method for using a water-based coating made from graphene glass powder, characterized in that: The graphene glass powder water-based coating comprises, by weight, the following components: 50-100 parts glass powder, 96-195 parts graphene oxide water slurry, 8-16 parts water-soluble resin binder, 1.6-3.2 parts dispersant, 32-64 parts water, and 0.8-1.6 parts reducing agent. A water-based graphene oxide slurry with a solid content of 3-5 wt%, a sheet size of 3-40 μm, and a carbon-to-oxygen ratio of 1.1-1.5:1 was prepared. Preparation of a water-soluble resin premix of glass powder: Weigh out 50-100 parts by weight of silica glass powder, 0-50 parts by weight of titanium dioxide glass powder, 0-35 parts by weight of alumina glass powder, 0-15 parts by weight of bismuthate glass powder, and 0-15 parts by weight of borosilicate metal salt glass powder. Melt them at a high temperature of 400-600℃ to form an amorphous eutectic. Grind and pulverize the eutectic into glass powder with a particle size of 5-10μm and a melting point of 200-500℃. Mix 8-16 parts by weight of water-soluble resin binder with 32-64 parts by weight of water and 1.6-3.2 parts by weight of dispersant evenly. Add the fully mixed glass powder with a melting point of 200-500℃, weigh out 50-100 parts by weight of glass powder, mix evenly, and obtain the water-soluble resin premix of glass powder. 96-195 parts of the graphene oxide aqueous slurry and 0.8-1.6 parts of reducing agent were mixed at 1200 r / min and 50°C for 0.5 h for weak reduction. The glass powder water-soluble resin premix was then added and mixed at 1200 r / min and cooled to room temperature to obtain a graphene glass powder water-based coating. In use, a substrate with a temperature resistance of 200℃ or higher is selected. The surface rust and stains are removed by sanding with sandpaper, and after rinsing with deionized water and drying, the prepared graphene glass powder water-based coating is evenly sprayed onto the surface of the substrate. Then, it is baked and cured. During the curing process, the temperature is increased from room temperature to 100℃ at a rate of 10℃ / min and held for 10 minutes. Then, the temperature is increased from 100℃ to 200℃ at a rate of 10℃ / min and held for 10 minutes. Finally, the temperature is increased to 300-500℃ at a rate of 10℃ / min and held for 20 minutes. After cooling, the graphene glass powder water-based coating is obtained.

2. The method of using a water-based graphene glass powder coating according to claim 1, characterized in that: The graphene oxide was prepared using the modified Hummers method.

3. The method of using a water-based graphene glass powder coating according to claim 1, characterized in that: The water-soluble resin adhesive is one or more of water-based polyurethane resin, water-based acrylic resin, water-based alkyd resin, water-based polyester resin, and water-based epoxy resin; the reducing agent is one or more of hydrazine hydrate, vitamin C, and glucose.

4. The method of using a water-based graphene glass powder coating according to claim 1, characterized in that: The glass powder, water-soluble resin binder, dispersant and water are compounded and then thoroughly mixed at 500 r / min for 0.5 h before use.