TWI639691B - Nano carbon material heat dissipation material manufacturing method - Google Patents

Abstract

The invention comprises the following steps: (A) preparing a water-soluble resin, a heat-conductive filler, a nano-carbon material and a surfactant, wherein the nano-carbon material comprises graphene and At least one of the carbon nanotubes, the surfactant comprising at least one of a wetting agent and a dispersing agent; (B) adding the surfactant to the water-soluble resin; (C) the surfactant containing the surfactant The heat conductive filler and the nano carbon material are added to the water-soluble resin, and the water-soluble resin, the heat-conductive filler, and the nano-carbon material are sufficiently mixed; and (D) the water-soluble resin is cured to complete the production of the heat-dissipating material. Thereby, the heat conductive filler and the nano carbon material are dispersed in the water-soluble resin to enhance the heat dissipation effect of the water-soluble resin.

Description

Nano carbon material heat dissipation material manufacturing method

The invention relates to a method for manufacturing a heat dissipating material, in particular to a method for manufacturing a heat dissipating material containing nano carbon materials.

With the advancement of technology, the performance requirements for various devices are becoming more stringent. Under the guidance of high performance products, general products need to be executed under high power. However, devices in high power operation are often accompanied by poor heat dissipation. Commonly used techniques to solve the problem of product heat dissipation include liquid cooling, air cooling, installation of heat dissipation structure, production of materials with high thermal conductivity materials, and application of heat dissipation materials at the heat dissipation interface of the device. Among them, the application of the heat dissipating material on the surface of the device is a simple and effective and relatively low-cost heat dissipation method, and has been widely used at present. However, this heat dissipation method has a certain improvement space in terms of heat dissipation.

Graphene and carbon nanotubes are novel nanomaterials, and the biggest problem in their application is how to mix and disperse with polymer substrates, thereby reflecting the excellent physical properties of graphene or carbon nanotubes. Due to its surface energy and high specific surface area, rice materials often have problems of uneven agglomeration and dispersion during mixing, and if they can improve the mixing of graphene or carbon nanotube materials in polymer substrates. The dispersion effect will contribute to the display of excellent physical properties (conductivity, heat conduction, mechanical strengthening, etc.) of nano carbon materials.

Therefore, at present, the industry needs a method for manufacturing a heat-dissipating material containing nano carbon materials, dispersing a heat-conducting filler and a nano-carbon material in a material, and preparing a heat-dissipating material that meets the needs of the industry through a simple preparation process.

In view of the above disadvantages of the prior art, the main object of the present invention is to provide a method for fabricating a heat-dissipating material containing nano carbon materials. The heat-conductive filler in the water-soluble resin can be used as a main medium for heat conduction, and the filled nano carbon material can be used as The thermal bridging medium between the thermally conductive fillers provides a good heat dissipation effect due to the high heat transfer coefficient of the thermally conductive filler and the nano carbon material.

In order to achieve the above object, according to one aspect of the present invention, a method for fabricating a heat-dissipating material containing a nano-carbon material is provided, the steps comprising: (A) preparing a water-soluble resin, a heat-conductive filler, a nano-carbon material, and a a surfactant, wherein the nano carbon material comprises at least one of graphene and a carbon nanotube, the surfactant comprising at least one of a wetting agent and a dispersing agent; (B) adding the water-soluble resin a surfactant; (C) adding the heat conductive filler and the nano carbon material to the water-soluble resin containing the surfactant, and thoroughly mixing the water-soluble resin, the heat conductive filler, and the nano carbon material; The curing of the heat dissipating material is completed by curing the water-soluble resin.

In the above, the humectant is an anionic surfactant, and the component of the humectant comprises sodium 1,4-dihexyl sulfosuccinate (C ₁₆ H ₂₉ O ₇ NaS); the weight percentage of the humectant is not more than 10%.

In the above, the dispersing agent is a cationic surfactant, and the component of the dispersing agent comprises tetrabutylammonium chloride (C ₄ H ₁₂ ClN); the dispersing agent is not more than 10% by weight.

In the above, the thermally conductive filler may comprise a plurality of ceramic particles having a particle diameter of not more than 10 micrometers; the thermally conductive filler may be made of at least one of aluminum nitride, aluminum oxide, thermal conductive carbon black, and ethyl cellulose.

In the above, the weight percentage of the heat conductive filler is 10% to 50%; and the weight percentage of the nano carbon material is not more than 10%.

In the above, the water-soluble resin is an epoxy resin.

In the above, the step (C) can be sufficiently mixed using a vacuum defoaming technique, a colloidal ball milling technique or a homogeneous stirring technique.

The invention relates to a method for preparing a heat-dissipating material containing nano carbon materials, wherein the heat-conductive filler in the water-soluble resin can serve as a main medium for heat conduction, and filling the nano-carbon material can serve as a heat bridge medium between the heat-conductive fillers ( The thermal-bridging material) provides a good heat dissipation effect because both the thermally conductive filler and the nanocarbon material have a high heat transfer coefficient. Further, by adding sodium 1,4-dihexyl sulfosuccinate and tetrabutylammonium chloride to the water-soluble resin, the wettability and dispersion of the nanocarbon material in the water-soluble resin can be enhanced. To prevent the nano carbon material from being uniformly dispersed in the water-soluble resin due to the agglomeration effect, to ensure the effect of the nano carbon material as a heat bridge medium, the heat dissipating material of the present invention is advantageous for enhancing the heat dissipation effect on the industry. The use of considerable economic improvements.

The above summary and the following detailed description and drawings are The manner, means and efficacy of the present invention for achieving the intended purpose can be further explained. Other objects and advantages of the present invention will be described in the following description and drawings.

S101-S104‧‧‧Steps

100‧‧‧heating materials

200‧‧‧heating items

1‧‧‧Water-soluble resin

2‧‧‧ Thermally conductive filler

3‧‧‧Nano carbon material

The first figure is a flow chart of a method for manufacturing a heat-dissipating material containing a nano carbon material according to the present invention; the second figure is a schematic view of an application form of a heat-dissipating material containing a nano-carbon material according to the present invention; EXAMPLES The distribution of nanocarbon materials in various solutions at different times.

The embodiments of the present invention are described by way of specific examples, and those skilled in the art can readily appreciate the advantages and effects of the present invention from the disclosure herein.

Please refer to the first figure, which is a flow chart of a method for manufacturing a nano-carbon material heat-dissipating material according to the present invention. As shown in the figure, a method for manufacturing a nanocarbon-containing heat dissipating material according to the present invention comprises the steps of: (A) preparing a water-soluble resin, a heat-conductive filler, a nano-carbon material, and a surfactant, wherein The nano carbon material comprises at least one of graphene and a carbon nanotube, the surfactant comprising at least one of a wetting agent and a dispersing agent S101; (B) adding the surfactant S102 to the water-soluble resin; C) adding the heat conductive filler and the nano carbon material to the water-soluble resin containing the surfactant, and the water-soluble resin, the heat conductive filler, and The nano carbon material is sufficiently mixed with S103; (D) the water-soluble resin is cured to complete the production of the heat dissipating material S104.

Example:

Please refer to the second figure, which is a schematic diagram of an application aspect of a heat-dissipating material containing nano carbon materials. As shown in the figure, in an embodiment of the method for manufacturing the heat dissipating material 100, the heat dissipating material 100 is applied to a heat dissipating material 200 to provide a heat dissipating effect, and the component of the heat dissipating material 100 comprises a water soluble resin. A thermally conductive filler 2 filled in the water-soluble resin 1, a nanocarbon material 3 filled in the water-soluble resin 1, and a surfactant component not shown in the drawing. The second figure represents the thermally conductive filler 2 in a white circular pattern and represents the nanocarbon material 3 in a black circular pattern. Hereinafter, specific embodiments of the present invention will be described with reference to the flowchart of the first drawing.

First, in this step S101, the water-soluble resin 1, the thermally conductive filler 2, the nanocarbon material 3, and the raw material of the surfactant are prepared in advance. In the present embodiment, the water-soluble resin 1 is a water-soluble epoxy resin which contains two main components such as a base agent and a curing agent which have not been mixed in the preparation step. The heat dissipating material 100 may be a micro- or nano-scale high thermal conductivity material, such as a mixture of one or more of aluminum nitride, aluminum oxide, thermally conductive carbon black, and ethyl cellulose to provide primary heat transfer. way. In some embodiments, the thermally conductive filler 2 may specifically comprise a plurality of ceramic particles of aluminum nitride particles, alumina particles, or the like having a particle diameter of not more than 10 micrometers, but is not limited by this embodiment. The nanocarbon material 3 comprises a mixture of one or more of an oligo-graphene, a single-walled carbon nanotube, and a multi-walled carbon nanotube, and can serve as a thermal bridging medium between the thermally conductive fillers 2 (thermal-bridging) Material). In some embodiments, the oligo-graphene has a thickness of less than 5 nm and a lateral dimension of between 0.1 and 5 microns, but is not limited to such graphene material. The surfactant comprises a wetting agent and a dispersing agent, and the wetting agent can improve the hydrophilicity of the nano carbon material 3 in an aqueous solution, for example, the component comprising 1,4-dihexyl sulfosuccinate sodium salt (C ₁₆ An anionic surfactant of H ₂₉ O ₇ NaS); the dispersant can improve the dispersibility of the nano carbon material 3 in an aqueous solution, thereby avoiding a significant agglomeration of the nano carbon material 3 in an aqueous solution, this embodiment As the dispersant, for example, a cationic surfactant containing tetrabutylammonium chloride (C ₄ H ₁₂ ClN) may be used.

Next, a surfactant may be added to the water-soluble resin 1 in step S102. In detail, this step is to use the base agent of the water-soluble resin 1, which is in an unsolidified state which is in the form of a gel or a paste in this step. In this step, at least one of the humectant and the dispersing agent of the surfactant may be added to the base agent of the water-soluble resin 1, and the preferred weight percentage of the humectant and/or the dispersing agent is not more than 10%, but the ratio of the humectant and/or the dispersant can be adjusted in different embodiments, and is not limited to the contents disclosed herein.

Further, in the step S103, the heat conductive filler 2 and the nano carbon material 3 may be added to the water-soluble resin 1 containing the surfactant, and the water-soluble resin 1, the heat conductive filler 2 and the nanometer may be added. Carbon material 3 is thoroughly mixed, the guide The weight percentage of the hot filler 2 is, for example, 10 to 50%, and the weight percentage of the nanocarbon material 3 is, for example, not more than 10%, but is not limited thereto. Wherein, in step S104, the water-soluble resin 1, the heat-conductive filler 2, the nano-carbon material 3 and the surfactant may be sufficiently mixed using a vacuum defoaming technique, a colloidal ball milling technique or a homogeneous stirring technique, but not Technology is limited.

Please refer to the third figure, which is a distribution state of nano carbon materials in various solutions at different times according to an embodiment of the present invention. Wherein (1) is an aqueous solution containing 0.05% sodium sulfouccinate 1,4-dihexyl ester (wetting agent) and 1% tetrabutylammonium chloride (dispersant) containing the nano carbon material 3. The indicator (2) is an aqueous solution containing the sodium dodecylbenzenesulfonate (SDBS) dispersant containing the nano carbon material 3, and the label (3) is added with 2% SDBS dispersant. An aqueous solution containing the nanocarbon material 3, and (4) is an aqueous solution containing the nanocarbon material 3, which is a generally more common dispersant, without any surfactant. The third graph (a) shows the state in which the four aqueous solutions have just been blended, and the third graph (b) shows the state in which the four aqueous solutions are allowed to stand for 4 hours. From the comparison between the third figure (a) and the third figure (b), the nano carbon materials 3 are uniformly distributed in the aqueous solution when the four aqueous solutions are just finished, but after a period of standing, the In the aqueous solution (2), (3) of SDBS and the aqueous solution (4) not containing any surfactant, the nanocarbon material 3 is agglomerated and precipitated, but 1,4-dihexyl sulfosuccinate is added. In the aqueous solution (1) of the sodium salt and tetrabutylammonium chloride, the nano carbon material 3 is still in a state of uniform distribution. Thus, it is known that the sodium 1,4-dihexyl sulfosuccinate and the tetrabutylate are added in this embodiment. Ammonium chloride can indeed be more than normal interfacial activity The agent enhances the dispersibility of the nanocarbon material 3, so that the nanocarbon material 3 is prevented from being uniformly dispersed in the water-soluble resin 1 to affect the heat conduction performance.

After the foregoing steps are completed, the water-soluble resin 1 can be cured in step S104 to complete the fabrication of the heat-dissipating material 100. In this step, for example, a curing agent can be added to the base agent of the water-soluble resin 1 at a ratio of 1 to 1, that is, the heat-dissipating material 100 can be produced in a non-solidified state. In addition, as shown in the application form of the second figure, the prepared heat dissipating material 100 can be coated on the surface of the object to be heat-dissipated 200, and the heat dissipating material 100 is rotated by natural shading or heat curing. It is solid and has a thickness of, for example, 10 micrometers to 60 micrometers, but not limited thereto, thereby providing a better heat dissipation effect on the heat dissipation surface of the article to be heat-dissipated 200.

Hereinafter, an embodiment will be described in conjunction with the above description, and a method of manufacturing the heat dissipating material 100 of the present invention will be specifically described. First, the base agent of the water-soluble epoxy resin is diluted in a ratio of 3:1 to an aqueous solution containing a wetting agent and a dispersing agent (the ratio of the base agent to the aqueous solution is 3 to 1) to form a gelatinous matrix having a total weight of 30 g. Wherein the wetting agent is 0.05% sodium 1,4-dihexyl sulfosuccinate and the dispersing agent is 1% tetrabutyl chloride. Then, alumina particles (30%) having a particle diameter of 0.5 μm are added as a heat conductive filler 2 to the above-mentioned colloidal matrix, and 2% graphene and 2% multi-walled carbon nanotubes are added as nano carbon material 3 to the planet. The above-mentioned raw materials are thoroughly mixed by a vacuum deaerator. Finally, the above-mentioned raw materials are added to the curing agent of the water-soluble epoxy resin in a ratio of 1:1 and thoroughly mixed to complete the production of the heat dissipating material 100. When you want to use it, you can apply a rod to coat the heat sink material 100. The heat dissipating material 100 can be turned into a solid state to provide heat dissipation effect by heating at 80 ° C for 30 minutes or natural shading on the item to be heat-dissipated.

Please refer to Table 1 for the comparison of the cooling effect of the heat dissipating material 100 with different proportions. The cooling effect is in accordance with the ASTM D5470 standard test method. A copper block is heated as a heater at a fixed power, and the heat dissipating material is uncoated and coated. The test piece to be tested of 100 is placed on the copper block for heating for a period of time, and the surface temperature is measured after the heat balance, thereby comparing the effect of heat dissipation. In this test, heating was performed at a power of 5 W for 4 hours, and the thickness of the heat dissipating material 100 was 40 μm. Under different conditions, the temperature at which the test piece not coated with the heat dissipating material 100 reaches the heat balance is not the same, but the range is generally between 60 and 80 ° C, and the cooling effect in the above table is the same. Under heating conditions, there is a difference between the temperature of the test piece to be tested coated with the heat dissipating material 100 and the test piece to be tested that is not coated with the heat dissipating material 100 after heat balance. It can be seen from the test results that the heat dissipating material 100 provides a heat dissipation effect of 4 ° C in the state where no surfactant is added, and is added with 0.05% sodium 1,4-dihexyl sulfosuccinate and 1% tetrabutylate. The cooling effect after the ammonium chloride can be increased to 6.45 ° C, and if the proportion of the nano carbon material 3 is further increased, the cooling effect can be raised to 9.28 ° C. It can be seen that the heat dissipating material 100 of the embodiment can provide an effective heat dissipating effect, and the addition of the surfactant can also improve the heat dissipating effect of the heat dissipating material 100.

The invention provides a method for preparing a heat-dissipating material containing nano carbon materials, wherein a water-soluble resin is used as a base material, and a ceramic filler having a particle diameter of less than 10 μm is added to the water-soluble resin, and a humectant (for example, sulfo amber) is added. Acid 1,4-dihexyl ester sodium salt), dispersant (such as tetrabutylammonium chloride) to improve the wettability of nano-carbon materials such as graphene and carbon nanotubes and dispersion in water-soluble resin Therefore, the ceramic filler can be used as the main heat dissipation medium in the water-soluble resin, and the nano-carbon material is used as a bridging material between the ceramic fillers to realize a high-efficiency heat-dissipating material, and the heat-dissipating material of the invention can effectively improve the heat dissipation. The effect can be directly applied to the heat dissipating component, making it more widely used in future applications.

The above-described embodiments are merely illustrative of the features and effects of the present invention and are not intended to limit the scope of the technical scope of the present invention. Any familiar with this Modifications and variations of the above-described embodiments may be made by those skilled in the art without departing from the spirit and scope of the invention. Therefore, the scope of protection of the present invention should be as set forth in the scope of the claims described below.

Claims (10)

The invention comprises the following steps: (A) preparing a water-soluble resin, a heat-conductive filler, a nano-carbon material and a surfactant, wherein the nano-carbon material comprises graphene and At least one of the carbon nanotubes, the surfactant comprising at least one of a wetting agent and a dispersing agent; (B) adding the surfactant to the water-soluble resin; (C) the surfactant containing the surfactant The heat conductive filler and the nano carbon material are added to the water-soluble resin, the water-soluble resin, the heat-conductive filler and the nano-carbon material are thoroughly mixed; and (D) the water-soluble resin is cured to complete the production of the heat-dissipating material, wherein The dispersant is a cationic surfactant, and the component of the dispersant comprises tetrabutylammonium chloride. The method for producing a nanocarbon-containing heat dissipating material according to claim 1, wherein the humectant is an anionic surfactant, and the component of the humectant comprises 1,4-dihexyl sulfosuccinate. Sodium salt. The method for producing a nanocarbon-containing heat dissipating material according to claim 1 or 2, wherein the humectant has a weight percentage of not more than 10%. The method for producing a nanocarbon-containing heat dissipating material according to claim 1, wherein the dispersing agent has a weight percentage of not more than 10%. The method for fabricating a nanocarbon-containing heat dissipating material according to claim 1, wherein the thermally conductive filler comprises a plurality of ceramic particles having a particle diameter of not more than 10 μm. The method for producing a nanocarbon-containing heat dissipating material according to claim 1, wherein the thermally conductive filler is made of at least one of aluminum nitride, aluminum oxide, thermally conductive carbon black, and ethyl cellulose. The method for manufacturing a nanocarbon-containing heat dissipating material according to claim 1, wherein the thermally conductive filler has a weight percentage of 10% to 50%. The method for producing a nanocarbon-containing heat dissipating material according to claim 1, wherein the nano carbon material has a weight percentage of not more than 10%. The method for producing a nanocarbon-containing heat dissipating material according to claim 1, wherein the water-soluble resin is an epoxy resin. The method for producing a nanocarbon-containing heat dissipating material according to claim 1, wherein the step (C) is sufficiently mixed by a vacuum defoaming technique, a colloidal ball milling technique or a homogeneous agitation technique.