CN116790118B - Graphene high-heat-conductivity composite material, preparation method thereof and high-heat-conductivity gasket - Google Patents
Graphene high-heat-conductivity composite material, preparation method thereof and high-heat-conductivity gasket Download PDFInfo
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Abstract
The invention provides a graphene high-heat-conductivity composite material, a preparation method thereof and a high-heat-conductivity gasket, and relates to the field of composite materials. The graphene high-heat-conductivity composite material comprises a coating material and a high-molecular resin material, wherein the coating material comprises the following components in percentage by mass: 0.1 to 2.0 percent of graphene, 41.2 to 55.2 percent of graphite, 11.7 to 37.7 percent of dispersion medium, 11.8 to 18.8 percent of aqueous coating solution, 0.1 to 5.0 percent of boron nitride, 0.5 to 2.0 percent of surface coating agent and 0.2 to 0.5 percent of air wetting and draining agent. The prepared heat-conducting composite material has good heat-conducting property and good mechanical property, the heat-conducting material does not need to be granulated, can be directly processed for the second time, and the high heat-conducting gasket formed by injection molding has good heat-conducting property and mechanical property.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a graphene high-heat-conductivity composite material, a preparation method thereof and a high-heat-conductivity gasket.
Background
With the continuous innovation of electronic technology products, the light weight and miniaturization aggregation of electronic products greatly improve the power of the electronic products, and the arrangement of electronic elements is more compact, so that high-quality heat conducting materials with excellent heat conducting performance are increasingly required to avoid the situation that the safety and performance of the electronic products are seriously affected by the heat aggregation effect of electronic equipment.
Graphene is a material with excellent heat conduction effect, the structure of the graphene is very stable, the connection between carbon atoms in the graphene is very flexible, and the graphene has higher in-plane heat conduction coefficient compared with the traditional metal materials such as copper, aluminum and the like. In addition, graphene has low density, good thermal stability and good mechanical property, so that graphene is doped in other heat conducting materials, the heat conducting property of the material can be improved, and the mechanical property of the material can be improved to a certain extent.
At present, graphene doped heat conducting materials are produced by uniformly filling graphene into a high polymer resin material. For example, a preparation method of a heat-conducting plastic disclosed in chinese patent application publication No. CN115304811a, which adopts graphene and plastic powder to mix directly in a solvent; as disclosed in chinese patent application publication No. CN115536012a, a preparation method thereof, and a composite heat conductive material, a graphene oxide slurry containing a polar solvent is mixed with a polymer soluble in the polar solvent; according to the graphene heat conduction material and the manufacturing method thereof disclosed in the Chinese patent application with the publication number of CN114131783A, solid raw materials are rolled into powder and then mixed with various liquid raw materials, and then the mixture is granulated to form the graphene heat conduction material.
However, the large amount of graphene can cause the material cost to rise in a multiple way, but only a small amount of graphene is doped, and it is difficult to increase good heat conduction performance and mechanical property for the existing material. Therefore, a graphene heat conduction material with good economic benefit and complete heat conduction performance and mechanical performance is urgently needed.
Disclosure of Invention
The invention provides a graphene high-heat-conductivity composite material, a preparation method thereof and a high-heat-conductivity gasket, which adopt a simple preparation process, can ensure high-efficiency heat conductivity, improve the mechanical property of the composite material, and the preparation process is safe and environment-friendly and reduces the cost.
The first aspect of the invention provides a graphene high-heat-conductivity composite material, which comprises a coating material and a high-molecular resin material, wherein the coating material comprises the following components in percentage by mass: 0.1 to 2.0 percent of graphene, 41.2 to 55.2 percent of graphite, 11.7 to 37.7 percent of dispersion medium, 11.8 to 18.8 percent of aqueous coating solution, 0.1 to 5.0 percent of boron nitride, 0.5 to 2.0 percent of surface coating agent and 0.2 to 0.5 percent of air wetting and draining agent.
Optionally, the graphene high thermal conductivity composite further comprises glass fibers.
Optionally, the polymeric resin material comprises one or more of the following: PA66, ABS758, or PET56151.
Optionally, the graphite is flake graphite with 100-500 meshes, and the dispersion medium is deionized water.
Optionally, the aqueous coating solution is an EVA emulsion.
Optionally, the surface coating agent is one or more of the following: polyvinylpyrrolidone, high molecular weight cellulose, polyethylene oxide or polyvinyl alcohol.
Optionally, the air wet drain agent is one or more of the following: surfactant 104PG or silicone 510.
According to a second aspect of the present invention, there is provided a method for preparing a graphene high thermal conductivity composite material, the method comprising the steps of:
S1, preparing a coating material, which comprises the following steps:
S1-1, sequentially adding an air wetting draining agent, a water-based coating solution and a surface coating agent into deionized water under the condition of stirring, and keeping stirring until the solution is in a transparent state to obtain a dispersion liquid for later use;
S1-2, sequentially adding graphite and boron nitride into stirring equipment, starting the stirring equipment to stir for 0.5-1 h, adding graphene, continuously stirring for 1.5-2 h, adding the dispersion liquid, stirring for 2-2.5 h at 75-85 ℃, vacuumizing, keeping the vacuum degree below 0.05MPa, and continuously stirring for 1.0-1.5 h at the temperature;
S1-3, drying the product prepared in the step S1-2 for 4.5-5 hours at the temperature of 75-80 ℃ under the vacuum degree of below 0.06MPa, and then crushing for 1.0-1.5 hours to obtain the coating material;
s2, preparing a graphene high-heat-conductivity composite material: mixing the coating material and the high polymer resin material, and placing the mixture into mixing equipment at a stirring rate of 80-100 r/min, and stirring at 100-110 ℃ for 8-10 min, thereby obtaining the graphene high-heat-conductivity composite material.
Optionally, the step S2 further comprises adding glass fibers to the mixing device and stirring.
According to a third aspect of the present invention there is provided a high thermal conductivity gasket prepared by: the graphene high-heat-conductivity composite material according to the first aspect is put into an injection molding machine, and an injection molding process is started, so that the high-heat-conductivity gasket is obtained.
The above-mentioned three patent documents and the prior art heat conductive materials not only use a large amount of graphene or noble metal, resulting in higher production cost of the materials, but also affect the mechanical properties of the materials if low-priced fillers are used for reducing the cost, so that the materials cannot be widely used because of single use. And a large amount of organic solvents or polar solvents, such as ethanol, diethyl ether, isopropanol or acetone, are used in the production process, so that a large amount of VOC (volatile organic compounds) is discharged, which is not beneficial to environmental protection. In addition, the method is to directly blend the graphene and the resin material to prepare the composite material, and even if other materials exist, the graphene and the resin material are blended or added into the system during blending, so that the final heat-conducting composite material is likely to be fixed in structure and difficult to reprocess, and the graphene and the resin material are likely to be unevenly mixed in the preparation process, thereby improving the production difficulty.
According to the graphene high-heat-conductivity composite material, the preparation method thereof and the high-heat-conductivity gasket, flake graphite with specific mesh number is selected, and the graphite can play a role in self-lubrication and arrangement in the preparation process to form a graphite skeleton, so that only a small amount of graphene and boron nitride are added as fillers of skeleton gaps, the heat conductivity of a product can be ensured, the cost can be reduced, and the mechanical property of the material is not reduced. According to the application, the aqueous coating solution with low glass transition temperature is selected, and the surface coating agent is a polymer material with strong hydrophilicity and high elastic modulus, so that the coated graphene and graphite can be tightly adhered together, the internal air can be removed, dust emission is avoided, and the powder can be directly molded, such as injection molding and the like, without granulating after the coating agent is mixed and compounded with the polymer resin material. The composite material prepared by the application is convenient for secondary processing, is beneficial to the molding of the material, and the molded material can not influence the mechanical property of the material.
The graphene high-heat-conductivity composite material provided by the invention has wide application, can be used as a gasket, and can be widely applied through other forming processes. Furthermore, after the glass fiber is added, the material has good compatibility with the glass fiber, less than 10% of the glass fiber is added, the fiber is not floated, and meanwhile, the mechanical property of the material can be improved by adding the glass fiber. The method provided by the invention adopts deionized water as a dispersion medium to coat graphite, and has zero VOC emission in the production process, safety and environmental protection.
Detailed Description
Reference will now be made in detail to various embodiments of the invention, examples of which are described below. While the invention will be described in conjunction with the exemplary embodiments thereof, it will be understood that the present description is not intended to limit the invention to those exemplary embodiments. On the other hand, the present invention is intended to cover not only the exemplary embodiments of the present invention, but also various alternatives, modifications, equivalents and other embodiments, which may be included within the spirit and scope of the invention as defined by the appended claims.
Hereinafter, exemplary embodiments of the present invention will be described in detail. The specific structures and functions described in the exemplary embodiments of the present invention are for illustrative purposes only. Embodiments of the inventive concept according to the present invention may be embodied in various forms and it should be understood that they should not be construed as limited to the exemplary embodiments described in the exemplary embodiments, but include all modifications, equivalents, or alternatives falling within the spirit and scope of the invention.
Throughout the specification, the terminology used herein is for the purpose of describing various exemplary embodiments only and is not intended to be limiting. It will be further understood that the terms "comprises," "comprising," "includes," "including" and the like, when used in this exemplary embodiment, specify the presence of stated features, steps, operations, or elements, but do not preclude the presence or addition of one or more other features, steps, operations, or elements.
The graphene powder mentioned in the invention is commercially available graphene powder with a carbon content of more than 99.95% and less than 10 layers, and all other used medicines without special description are purchased from Siya chemical technology (Shandong) limited company.
In one aspect of the present application, there is provided a graphene high thermal conductive composite material (hereinafter also referred to as "high thermal conductive composite material" or "composite material" for convenience of description, which is practically equivalent to the graphene high thermal conductive composite material mentioned in the present application), the composite material comprising a clad material and a high molecular resin material, the clad material comprising the following components in mass percent: 0.1 to 2.0 percent of graphene, 41.2 to 55.2 percent of graphite, 11.7 to 37.7 percent of dispersion medium, 11.8 to 18.8 percent of aqueous coating solution, 0.1 to 5.0 percent of boron nitride, 0.5 to 2.0 percent of surface coating agent and 0.2 to 0.5 percent of air wetting and draining agent.
It should be noted that the above components are 100% by weight of the total coating material. In discussing the mass percentages of the clad material and the polymer resin material, the total mass of the two materials is calculated as 100%. For convenience of description, the mass percentages of the respective components are listed in table 1.
Table 1: the coating material comprises the following components in percentage by mass
| Sequence number | Material | Weight percent |
| 1 | Graphene | 0.1～2.0％ |
| 2 | Graphite | 41.2～55.2％ |
| 3 | Dispersing medium | 11.7～37.7％ |
| 4 | Aqueous coating solution | 11.8～18.8％ |
| 5 | Boron nitride | 0.1～5.0％ |
| 6 | Surface coating agent | 0.5～2.0％ |
| 7 | Air wetting and draining agent | 0.2～0.5％ |
Further, in some embodiments, the high thermal conductive composite material provided by the invention may further include a reinforcing material, for example, the reinforcing material may be glass fiber, and in the case of using glass fiber, the addition amount of the glass fiber is less than 10% of the total mass of the high thermal conductive composite material, and the coating material and the polymer resin material of the invention have good compatibility with the glass fiber, so that the glass fiber added by less than 10% does not float, and the compounding condition is good. Thus, the mechanical properties of the material can be further improved by adding glass fibers. In addition, it should be noted that when glass fibers are included in the high thermal conductive material, the mass percentages of the clad material, the polymer resin material, and the glass fibers are discussed as being calculated by taking the total mass of the three substances as 100%.
In some embodiments of the present application, the polymer resin material may include one or more of PA (nylon) 66, ABS (acrylonitrile-butadiene-styrene copolymer) 758, or PET (polyethylene terephthalate) 56151. The polymer resin material is selected from the Dongguan Xin Heng rubber and plastic limited company, can be powder material and/or granular material, and has the particle size of 1-2 mm.
In some embodiments of the application, the graphite can be 100-500 mesh flake graphite, and the flake graphite with specific mesh number can be selected, so that the graphite can be self-lubricated and arranged in a system to form a framework during injection molding, and a lubricant is not required to be added separately. Through the formed graphite skeleton, the boron nitride and doped graphene can be added subsequently to serve as a filler of a skeleton gap, and the graphene has good heat conduction and mechanical properties, so that the skeleton can be supported, the mechanical properties of the graphite can be improved, the heat conduction property of the material can be further improved, and meanwhile, the production cost can be reduced.
The dispersion medium provided by the invention adopts deionized water, avoids adding an organic solvent in the preparation process, has zero VOC emission in the production process, is environment-friendly, and has safe and efficient production process.
In some embodiments of the application, the aqueous coating solution employed in the present application is an EVA (ethylene vinyl acetate) emulsion.
In some embodiments of the present application, the surface coating agent employs a high molecular material with strong hydrophilicity and high elastic modulus, while also being oleophilic and inorganic (graphite), such as one or more of the following: polyvinylpyrrolidone (PVP), high molecular weight cellulose, polyethylene oxide PEO or polyvinyl alcohol PVOH. The surface coating agent is used, so that the surface of the graphite can be completely coated, and the bonding between the graphite is tighter. Wherein, the high molecular weight cellulose can be hydroxypropyl methyl cellulose and/or hydroxyethyl cellulose with the molecular weight of 30-100 ten thousand Da. Further, in some embodiments of the application, the air wet drain agent may be one or more of the following: after the surfactant 104PG or the organic silicon 510 is added into the air wetting and draining agent, the air in the system can be drained, and the raw materials are prevented from reacting due to contact with oxygen in the air, so that the effect of the final product is prevented from being influenced.
Based on the above, the high heat conduction composite material is compounded by using the coating type material and the high polymer resin material, wherein the coating type material coats graphene and graphite by using materials such as a coating agent, a dispersion liquid and the like, so that the heat conduction performance and the mechanical performance of the material are improved, and then the coating type material is compounded with the high polymer resin material, so that the high heat conduction composite material with good mechanical performance and heat conduction performance is prepared.
Based on the second aspect of the present invention, the present invention also provides a preparation method of the graphene high thermal conductivity composite material, which includes two steps of preparation of the coating material and preparation of the graphene high thermal conductivity composite material, and the two steps will be described in detail below.
S1, preparing a coating type material, wherein the preparation of the coating type material comprises the following steps: s1-1, sequentially adding an air wetting draining agent, an aqueous coating solution and a surface coating agent into deionized water under the condition of stirring, and keeping stirring until the solution is in a transparent state to obtain a dispersion liquid for standby. Specifically, in the preparation process, deionized water is added into a reaction vessel, such as a large-sized reactor, a three-necked flask in a laboratory or the like, according to the proportion of the above materials, and stirred, and can be selected according to actual needs (such as the addition amount of the materials), which is not particularly limited in the present application. The stirring speed can be 350-450 r/min, the air wetting draining agent is added while stirring, the stirring is kept for 5-6 min, then the aqueous coating solution is added and the stirring is continued for 5-6 min, finally the surface coating agent is added into the system, the rotating speed is increased to 500-600 r/min, the stirring is kept for 1.5-2 h until the solution in the system is in a transparent state, and at the moment, the added coating agent can be completely dispersed. The process can be actually regarded as a preparation process of the coating liquid, and after the coating liquid is uniformly dispersed in the system, the coating liquid can be directly coated with graphite, boron nitride and graphene.
S1-2, sequentially adding graphite and boron nitride into stirring equipment, starting the stirring equipment to stir for 0.5-1 h, adding graphene, continuously stirring for 1.5-2 h, adding the dispersion liquid, stirring for 2-2.5 h at 75-85 ℃, vacuumizing, keeping the vacuum degree below 0.05MPa, and continuously stirring for 1.0-1.5 h at the temperature. The stirring device can be a planetary mixing device or other devices capable of stirring and mixing the materials, and the stirring speed of the stirring device can be kept between 15 and 20r/min.
S1-3, drying the product prepared in the step S1-3 for 4.5-5 hours at the temperature of 75-80 ℃ under the vacuum degree of below 0.06MPa, and then crushing for 1.0-1.5 hours to obtain the coating material. Specifically, after the vacuumizing time in the step S1-2 is over, the vacuumizing, heating and stirring processes are sequentially stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying box for drying, so that the vacuum degree is kept below 0.06MPa, the materials are baked and dried for 4.5-5.0 h at 75-80 ℃, and after the vacuum drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20-25 r/min, and crushing is carried out for 1.0-1.5 h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Next, S2, preparation of graphene high-thermal-conductivity composite material: mixing the coating material and the high polymer resin material, and placing the mixture into mixing equipment at a stirring rate of 80-100 r/min, and stirring at 100-110 ℃ for 8-10 min, thereby obtaining the graphene high-heat-conductivity composite material. The mixing device may be a kneader or the like capable of sufficiently mixing the materials. Therefore, the composite material with good heat conducting performance and high mechanical property and strength is obtained by compounding the coating material and the high polymer resin material.
Further, in some embodiments of the present application, the step S2 may further include adding glass fibers to the mixing apparatus and stirring after mixing the clad material and the polymer resin material in the mixing apparatus for 8 to 10 minutes, the addition amount of the glass fibers is not more than 10%, for example, 8%, 5%, etc., of the total mass of the clad material and the polymer resin material, and the stirring time may be, for example, 8 to 10 minutes. Therefore, the addition of the glass fiber can ensure that the mechanical property of the composite material is improved as much as possible under the condition of no fiber floating, the strength of the material is further enhanced, and the composite material can be ensured to have good thermal conductivity.
According to the method provided by the invention, the situation that graphene is difficult to mix due to direct contact with high polymer resin and a large amount of organic solvent is needed to promote mixing is avoided in the preparation process, the graphene, the graphite and the boron nitride are firstly blended and coated to form a stable skeleton structure, and then the stable skeleton structure is compounded with the high polymer resin material, so that the mechanical property of the material can be improved, the consumption of the graphene can be reduced, the heat conduction effect can be improved, and the deionized water is adopted as a dispersing agent, any organic solvent is not added in the reaction process, the reaction process is safe and environment-friendly, dust emission is avoided, and VOC emission can be avoided. Examples of preparing graphene high thermal conductivity composites using the methods of the present invention are provided below.
Example 1
Preparing a coating material: adding 35.02% deionized water (calculated by taking the total mass of the components required in the preparation process of the coating material as 100% and not described in detail below) into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.35% surfactant 104PG while stirring, keeping the stirring speed for 5min, adding 16.51% EVA emulsion and continuing stirring for 5min, adding 0.71% polyvinylpyrrolidone into the reaction container, increasing the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 47.17% of graphite and 0.12% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.12% of graphene to continuously stir for 1.5 hours after stirring for 0.5 hours at a stirring rate of 15r/min, then adding the dispersion, starting heating, stirring for 2 hours at 75 ℃, vacuumizing, and continuously stirring for 1 hour at the temperature and stirring rate under the environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: 60% of the coating material and 40% of the granular PA66 are mixed and put into a mixing device according to the mass percentage (as described above, the mass percentage is calculated by taking the total mass of the coating material and the high polymer resin material as 100%, and the description will not be repeated), and the mixture is stirred at the stirring rate of 80r/min for 8min at the temperature of 100 ℃, so that the graphene high thermal conductivity composite material is obtained.
Example 2
Preparing a coating material: adding 35.70% of deionized water in percentage by mass into a reaction container, starting stirring to enable the stirring speed to be 450r/min, adding 0.36% of organosilicon 510 while stirring, keeping the stirring speed for 6min, adding 14.42% of EVA emulsion and continuing stirring for 6min, then adding 1.20% of high molecular weight cellulose HBC and HPC into the reaction container, and improving the stirring speed to 600r/min, and continuing stirring for 2h until the solution in the system is in a transparent state to obtain a dispersion; adding 48.08% of graphite and 0.12% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.12% of graphene for continuous stirring for 2 hours after stirring for 1 hour at a stirring rate of 20r/min, then adding the dispersion, starting heating, stirring for 2.5 hours at 85 ℃, vacuumizing, and keeping the temperature and the stirring rate for continuous stirring for 1.5 hours under an environment with a vacuum degree of 0.04 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the baking and drying are carried out for 5 hours at 80 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotation speed is 25r/min, and crushing is carried out for 1.5h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 60% of coating material and 40% of granular PA66 by mass percent, and placing the mixture into mixing equipment to stir at 110 ℃ for 10min at a stirring rate of 100r/min, thereby obtaining the graphene high-heat-conductivity composite material.
Example 3
Preparing a coating material: adding 34.10 mass percent of deionized water into a reaction container, starting stirring to ensure that the stirring speed is 400r/min, adding 0.34 mass percent of surfactant 104PG while stirring, keeping the stirring speed for 6min, adding 13.78 mass percent of EVA emulsion, continuing stirring for 6min, adding 1.15 mass percent of polyethylene oxide into the reaction container, improving the stirring speed to 550r/min, and continuing stirring for 2h until the solution in the system is in a transparent state to obtain a dispersion; adding 45.92% of graphite and 4.59% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.11% of graphene for continuous stirring for 2 hours after stirring for 1.5 hours at a stirring rate of 17r/min, then adding the dispersion, starting heating, stirring for 2.5 hours at 80 ℃, vacuumizing, and keeping the temperature and the stirring rate for continuous stirring for 1.5 hours under the environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the baking and drying are carried out for 5 hours at 80 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotation speed is 25r/min, and crushing is carried out for 1.5h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 50% of coating material and 50% of powdery PA66 in percentage by mass, and placing the mixture into mixing equipment to stir for 10min at 105 ℃ at a stirring rate of 90r/min, thereby obtaining the graphene high-heat-conductivity composite material.
Example 4
Preparing a coating material: adding 34.10% of deionized water in percentage by mass into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.34% of surfactant 104PG in percentage by mass while stirring, keeping the stirring speed for 5min, adding 13.78% of EVA emulsion and continuing stirring for 5min, then adding 1.15% of polyvinyl alcohol into the reaction container, improving the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 45.92% of graphite and 4.59% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.11% of graphene for continuous stirring for 1.5 hours at a stirring rate of 15r/min, then adding the dispersion liquid, starting heating, stirring for 2 hours at 75 ℃, vacuumizing, and keeping the temperature and the stirring rate for continuous stirring for 1 hour under an environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 40% of coating material and 60% of powdery PA66 by mass percent, and placing the mixture into mixing equipment to stir at the stirring rate of 80r/min for 8min at the temperature of 100 ℃, thereby obtaining the graphene high-heat-conductivity composite material.
Example 5
Preparing a coating material: adding 34.90 mass percent of deionized water into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.35 mass percent of surfactant 104PG while stirring, keeping the stirring speed for 5min, adding 14.10 mass percent of EVA emulsion, continuing stirring for 5min, adding 1.18 mass percent of polyvinylpyrrolidone into the reaction container, increasing the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 47.00% of graphite and 2.35% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.12% of graphene for continuous stirring for 1.5 hours after stirring at a stirring rate of 15r/min, then adding the dispersion, starting heating, stirring at 75 ℃ for 2 hours, vacuumizing, and keeping the temperature and stirring rate for continuous stirring for 1 hour under an environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 55% of coating material and 45% of powdery PA66 in percentage by mass, and placing the mixture into mixing equipment to stir at the stirring rate of 80r/min for 8min at the temperature of 100 ℃, thereby obtaining the graphene high-heat-conductivity composite material.
Example 6
Preparing a coating material: adding 27.47 mass percent of deionized water into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.27 mass percent of surfactant 104PG while stirring, keeping the stirring speed for 5min, adding 16.48 mass percent of EVA emulsion, continuing stirring for 5min, adding 0.55 mass percent of polyvinylpyrrolidone into the reaction container, increasing the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 54.95% of graphite and 0.14% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.14% of graphene for continuous stirring for 1.5 hours after stirring at a stirring rate of 15r/min, then adding the dispersion, starting heating, stirring for 2 hours at 75 ℃, vacuumizing, and keeping the temperature and stirring rate for continuous stirring for 1 hour under an environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 55% of coating material and 45% of granular PA66 by mass percent, and placing the mixture into mixing equipment to stir at the stirring rate of 80r/min for 8min at the temperature of 100 ℃, thereby obtaining the graphene high-heat-conductivity composite material.
Example 7
Preparing a coating material: adding 34.90 mass percent of deionized water into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.35 mass percent of surfactant 104PG while stirring, keeping the stirring speed for 5min, adding 14.10 mass percent of EVA emulsion, continuing stirring for 5min, adding 1.18 mass percent of polyvinylpyrrolidone into the reaction container, increasing the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 47.00% of graphite and 2.35% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.12% of graphene for continuous stirring for 1.5 hours after stirring at a stirring rate of 15r/min, then adding the dispersion, starting heating, stirring at 75 ℃ for 2 hours, vacuumizing, and keeping the temperature and stirring rate for continuous stirring for 1 hour under an environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 40% of coating material and 60% of granular ABS758 in percentage by mass, and placing the mixture into mixing equipment to stir at the stirring rate of 80r/min for 8min at the temperature of 100 ℃, thereby obtaining the graphene high-heat-conductivity composite material.
Example 8
Preparing a coating material: adding 34.90 mass percent of deionized water into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.35 mass percent of surfactant 104PG while stirring, keeping the stirring speed for 5min, adding 14.10 mass percent of EVA emulsion, continuing stirring for 5min, adding 1.18 mass percent of polyvinylpyrrolidone into the reaction container, increasing the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 47.00% of graphite and 2.35% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.12% of graphene for continuous stirring for 1.5 hours after stirring at a stirring rate of 15r/min, then adding the dispersion, starting heating, stirring at 75 ℃ for 2 hours, vacuumizing, and keeping the temperature and stirring rate for continuous stirring for 1 hour under an environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: 40% of coating material and 60% of granular PET56151 in percentage by mass are mixed and put into mixing equipment to be stirred for 8min at the temperature of 100 ℃ at the stirring rate of 80r/min, so that the graphene high-heat-conductivity composite material is obtained.
Example 9
Preparing a coating material: adding 34.90 mass percent of deionized water into a reaction container, starting stirring to ensure that the stirring speed is 350r/min, adding 0.35 mass percent of surfactant 104PG while stirring, keeping the stirring speed for 5min, adding 14.10 mass percent of EVA emulsion, continuing stirring for 5min, adding 1.18 mass percent of polyvinylpyrrolidone into the reaction container, increasing the stirring speed to 500r/min, and continuing stirring for 1.5h until the solution in the system is in a transparent state to obtain a dispersion; adding 47.00% of graphite and 2.35% of boron nitride in percentage by mass into stirring equipment, starting stirring, adding 0.12% of graphene for continuous stirring for 1.5 hours after stirring at a stirring rate of 15r/min, then adding the dispersion, starting heating, stirring at 75 ℃ for 2 hours, vacuumizing, and keeping the temperature and stirring rate for continuous stirring for 1 hour under an environment with a vacuum degree of 0.05 MPa; after the vacuumizing time is over, the vacuumizing stirring and heating are stopped, the mixed materials in the stirring equipment are transferred into a baking tray, and then are put into a vacuum drying oven for drying, so that the vacuum degree is kept at 0.06MPa, the materials are baked and dried for 4.5 hours at 75 ℃, and after the vacuumizing drying time is over, the materials in the baking tray are poured into the stirring equipment again for crushing: stirring equipment is started, the rotating speed is 20r/min, and crushing is carried out for 1.0h through stirring, so that graphite powder with uniform coating size, namely the coating material, is obtained.
Preparing a graphene high-heat-conductivity composite material: mixing 50% of coating material and 40.9% of powdery PA66 by mass percent, putting the mixture into mixing equipment, stirring the mixture for 8 minutes at the temperature of 100 ℃ at the stirring rate of 80r/min, adding 9.1% of glass fiber by mass percent into the mixing equipment, and keeping the stirring rate for 8 minutes, thereby obtaining the graphene high-heat-conductivity composite material.
Performance test:
The graphene high thermal conductivity composite materials in the above examples 1 to 9 were directly placed into a material port of an injection molding machine, and were injection molded into sheet-shaped test pieces under the same technological parameters, and the thermal conductivity and mechanical properties thereof were tested by an experimental instrument, and the average value of 5 tests was taken as a final test value for each example sample, so as to obtain the thermal conductivity, tensile strength, bending elastic modulus and cantilever impact strength of the graphene high thermal conductivity composite materials prepared in each example, and specific experimental data are shown in table 2 below:
Table 2: examples test data
As can be seen from the test results in Table 2, the graphene high-thermal-conductivity composite material prepared by the preparation method of the graphene high-thermal-conductivity composite material has high thermal conductivity and excellent mechanical properties, and the coating material provided by the invention can be compounded with various polymer resin materials, can change the types of the polymer resin materials according to the specific application field, and has wide application fields. In addition, the graphene high-heat-conductivity composite material provided by the invention has good compatibility with glass fibers, and can improve the overall mechanical property of the material on the premise of ensuring the heat-conductivity effect after the glass fibers are added, and the addition amount of the glass fibers can be flexibly matched according to the needs, so that the ideal use performance is realized.
According to a third aspect of the present invention, there is provided a high thermal conductivity gasket, which is obtained by directly putting the graphene high thermal conductivity composite material of the first aspect into an injection molding machine, and starting an injection molding process. The injection molding process parameters may be, for example, the following parameters: feeding port temperature: the temperature of the charging barrel area is 60-80 ℃ which is higher than the melting temperature of the resin by 5 ℃, the temperature of each section from the rear area to the nozzle should be increased stepwise by 5 ℃, the injection pressure is 90-130 MPa, the back pressure is 30-50 MPa, and the rotating speed of the screw is 0.7-1.5 m/s. The graphene high-heat-conductivity composite material provided by the invention can be directly put into an injection molding machine for injection molding without reprocessing, and the prepared high-heat-conductivity gasket has good heat-conductivity and mechanical properties.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and their practical application to enable others skilled in the art to make or utilize the invention in various exemplary embodiments and with various alternatives and modifications. It is intended that the scope of the invention be defined by the claims appended hereto and their equivalents.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention. In the description of the present specification, the descriptions of the terms "one embodiment," "some embodiments," "examples," "particular examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Claims (9)
1. The graphene high-heat-conductivity composite material is characterized by comprising a coating material and a high-molecular resin material, wherein the coating material comprises the following components in percentage by mass: 0.1 to 2.0 percent of graphene, 41.2 to 55.2 percent of graphite, 11.7 to 37.7 percent of dispersion medium, 11.8 to 18.8 percent of aqueous coating solution, 0.1 to 5.0 percent of boron nitride, 0.5 to 2.0 percent of surface coating agent and 0.2 to 0.5 percent of air wetting and draining agent; the air wetting and draining agent is one or more of the following: surfactant 104PG or silicone 510.
2. The graphene high thermal conductivity composite of claim 1, further comprising a reinforcing material.
3. The graphene high thermal conductivity composite material according to claim 1 or 2, wherein the polymeric resin material comprises one or more of the following: PA66, ABS758, or PET56151.
4. The graphene high thermal conductivity composite material according to claim 1 or 2, wherein the graphite is 100-500 mesh flake graphite, and the dispersion medium is deionized water.
5. The graphene high thermal conductivity composite of claim 1 or 2, wherein the aqueous coating solution is an EVA emulsion.
6. The graphene high thermal conductivity composite of claim 1 or 2, wherein the surface coating agent is one or more of the following: polyvinylpyrrolidone, high molecular weight cellulose, polyethylene oxide or polyvinyl alcohol.
7. The preparation method of the graphene high-heat-conductivity composite material is characterized by comprising the following steps of:
S1, preparing a coating material, which comprises the following steps:
S1-1, sequentially adding an air wetting draining agent, a water-based coating solution and a surface coating agent into deionized water under the condition of stirring, and keeping stirring until the solution is in a transparent state to obtain a dispersion liquid for later use;
S1-2, sequentially adding graphite and boron nitride into stirring equipment, starting the stirring equipment to stir for 0.5-1 h, adding graphene, continuously stirring for 1.5-2 h, then adding the dispersion liquid, stirring for 2-2.5 h at 75-85 ℃, vacuumizing, and keeping the vacuum degree at 0.05
Keeping the temperature below MPa and continuously stirring for 1.0-1.5 h;
S1-3, drying the product prepared in the step S1-2 for 4.5-5 hours at the temperature of 75-80 ℃ under the vacuum degree of below 0.06MPa, and then crushing for 1.0-1.5 hours to obtain the coating material;
s2, preparing a graphene high-heat-conductivity composite material: mixing the coating material and the high polymer resin material, and placing the mixture into mixing equipment at a stirring rate of 80-100 r/min, and stirring at 100-110 ℃ for 8-10 min, thereby obtaining the graphene high-heat-conductivity composite material.
8. The method of preparing a graphene high thermal conductivity composite material according to claim 7, wherein step S2 further comprises adding glass fibers to the mixing device and stirring.
9. The high-heat-conductivity gasket is characterized by being prepared by the following steps: the graphene high thermal conductivity composite material according to any one of claims 1 to 6 is put into an injection molding machine, and an injection molding process is started, so that the high thermal conductivity gasket is obtained.
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| CN112708270A (en) * | 2021-02-01 | 2021-04-27 | 杭州本松新材料技术股份有限公司 | High-thermal-conductivity nylon-based composite material and preparation method thereof |
| CN113150541A (en) * | 2021-04-02 | 2021-07-23 | 浙江工业大学 | High-strength high-thermal-conductivity nylon composite material and preparation method thereof |
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| CN109265986A (en) * | 2018-09-25 | 2019-01-25 | 杭州本松新材料技术股份有限公司 | A kind of high thermal conductivity nylon composite materials |
| CN112708270A (en) * | 2021-02-01 | 2021-04-27 | 杭州本松新材料技术股份有限公司 | High-thermal-conductivity nylon-based composite material and preparation method thereof |
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