CN113416389A - Ultrahigh isotropic heat conduction material of epoxy two-dimensional sheet metal nano filler and preparation method thereof - Google Patents
Ultrahigh isotropic heat conduction material of epoxy two-dimensional sheet metal nano filler and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ultrahigh isotropic heat conduction material of an epoxy two-dimensional flaky metal nano filler and a preparation method thereof, wherein the material mainly comprises epoxy resin, the two-dimensional flaky metal nano filler, the two-dimensional flaky carbon series heat conduction filler and a diluent. According to the invention, two-dimensional flaky heat-conducting fillers are lapped in the epoxy resin matrix to form a three-dimensional heat-conducting network, so that the efficient lapping and efficient synergistic effect of the two-dimensional flaky metal nano-fillers are realized, the heat-conducting property of the obtained heat-conducting material or a product is greatly improved, and the three-dimensional flaky heat-conducting network has the characteristic of isotropic heat conduction.
Description
Technical Field
The invention belongs to the technical field of heat conducting materials, and particularly relates to an ultrahigh isotropic heat conducting material of an epoxy-based two-dimensional flaky metal nano filler and a preparation method thereof.
Background
The thermal management problem is more prominent due to the vigorous development of power density in the fields of microelectronics, photoelectricity, energy collection and the like. Insufficient heat dissipation can cause heat to build up in the electronic device, which overheating can reduce the useful life of the device, cause damage to the device, and even cause a fire. Therefore, in such fields, thermal management issues need to be optimized and solved. Therefore, the development of highly efficient thermally conductive materials and the realization of commercial applications of this type of thermal interface material are key to solving the thermal management problem.
The traditional thermal interface material is generally prepared by adding a thermal filler with better thermal conductivity into a polymer, mainly exists in the forms of thermal grease, thermal phase change materials and an adhesive, and is used for filling a gap between a radiator and an electronic device, so that the radiating efficiency is improved, and the service life of equipment is prolonged. The traditional thermal interface material has low thermal conductivity (usually 0.5-5 Wm)-1K-1In between), the heat filler is difficult to form a continuous and complete heat conduction network in the heat filler, and the heat transfer efficiency is low due to the existence of large air thermal resistance and interface thermal resistance. Such inefficient thermal interface materials are difficult to meet the heat dissipation requirements of dense high power electronic devices.
The key to preparing the thermal interface material with high thermal conductivity is to select the efficient heat-conducting filler and the efficient synergistic design between the fillers. Currently, high thermal conductivity fillers are mainly classified into three types, ceramic, metal and carbon-based fillers. Wherein, the ceramic filler (such as boron nitride, aluminum oxide, etc.) belongs to the insulating heat-conducting filler, and the heat transfer mechanism thereof belongs to phonon heat transfer. The metal filler and the carbon-based filler (such as graphene, carbon fiber, carbon nanotube and the like) have certain electrical conductivity, and the heat transfer of the metal filler and the carbon-based filler can be realized by electrons and phonons together. Thus, for thermal interface materials that do not have the insulation requirements, metal and carbon-based materials with high thermal conductivity are ideal filler choices.
Metal fillers such as gold, silver, copper, nickel, aluminum and the like have high intrinsic heat-conducting property and are often used as heat-conducting fillers in the field of heat management. However, high thermal conductivities are often difficult to achieve for polymer-pure metal filler systems. In order to improve the thermal conductivity of the system, two or more fillers are usually compounded to realize the synergistic interaction between the fillers.
Researchers have prepared thermally conductive materials by compounding High Density Polyethylene (HDPE) -copper powder (Cu) -carbon tubes (Arash, Badakhsh, Chan, et al, from morphology of attached copper/MWCNT fibers to thermal and mechanical characteristics of the present invention Polymer-matrix composites: An analytical and experimental study [ J ]. Journal of Applied Polymer Science,2017,134, 41 (45397)), co-milling copper and multi-wall carbon nanotubes with a ball mill, and then adding the milled composite powder as a composite thermally conductive filler to HDPE to prepare a thermally conductive Polymer-copper sheet-carbon tube composite material. Research shows that when the volume fraction of the filler reaches 10%, the thermal conductivity of the material can reach 1.09W/m.K, and the mechanical property is improved to a certain extent. There is a research on a method for preparing a polymer composite high thermal material by electrophoretically depositing a heat-conducting coating layer of copper particles and hexagonal boron nitride (hBN) on the surface of a carbon fiber fabric, then immersing the heat-conducting coating layer in resin, and carrying out hot-pressing curing molding. When the volume content of hBN/Cu reaches 2.84%, the material obtains a vertical thermal conductivity of 2.16W/m.K and an in-plane thermal conductivity of 6.14W/m.K (Xz A, Sk B, Chan W. enhancement of thermal conductivity of carbon fiber-recycled polymer composite with co-holder and boron nitride particles-scientific direct [ J ] Composites Part A: Applied Science and efficiency, 2019,121:449 Man 456.). In addition, a method for preparing the epoxy composite heat conduction material by filling the epoxy resin with the copper-aluminum ratio in a composite mode is researched. The effect of the copper/aluminum ratio on the thermal conductivity of the material was investigated by varying the copper/aluminum addition ratio (1 wt%, 2.5 wt% and 5.5 wt%). Researches show that the highest Thermal Conductivity of the system can reach 0.4985W/m.K, and the Thermal Conductivity of pure Epoxy can be improved by 9% by adding titanium dioxide powder on the basis (Saini A, Aseer J R. Experimental and Thermal Conductivity Analysis of Copper/aluminum cured Epoxy polymers).
As can be seen from the above, most of the polymer composite heat conduction materials filled with metal composite fillers at present utilize the synergistic effect of different heat conduction fillers to a certain extent, but the heat conductivity thereof is still low, and is usually difficult to be higher than 5W/m · K, and the heat conduction has anisotropy, and some and only some have good heat conduction performance in a certain direction, while the heat conduction performance in other directions is very poor, and is difficult to meet higher heat conduction standards and requirements, thereby limiting the product shape specification and application range of the materials thereof. In addition, in order to achieve better thermal conductivity, the raw materials with higher cost are generally selected, and the preparation method is more complicated and is not suitable for preparing the high-efficiency thermal interface material which can be commercially applied.
Therefore, if a polymer-based thermal conductive material with ultrahigh isotropic thermal conductivity is provided, the commercial application of the thermal interface material of the type can be greatly facilitated, and the contribution to solving the thermal management problem of subsequent industrial products is provided.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides an ultrahigh isotropic heat conduction material of an epoxy-based two-dimensional sheet metal nano filler and a preparation method thereof. According to the invention, two-dimensional flaky heat-conducting fillers are lapped in the epoxy resin matrix to form a three-dimensional heat-conducting network, so that the efficient lapping and efficient synergistic effect of the two-dimensional flaky metal nano-fillers are realized, the heat-conducting property of the obtained heat-conducting material or a product is greatly improved, and the three-dimensional flaky heat-conducting network has the characteristic of isotropic heat conduction.
In order to achieve the purpose, the invention adopts the technical scheme formed by the following technical measures.
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional flaky metal nano filler mainly comprises the following components in parts by weight:
wherein the average lamella thickness of the two-dimensional flaky metal nano filler is 100-500 nm, the average outer diameter is 10-100 μm,
the average lamella thickness of the two-dimensional flaky carbon-based heat-conducting filler is 10-500 nm, and the average outer diameter is 1-50 μm.
Generally, the epoxy resin can be selected from epoxy-based polymers that are common knowledge in the art and are commercially available, and can also be selected according to the actual use requirements and scenarios of the thermal conductive material. For better illustration of the present invention and to provide reference to several preferred embodiments, the epoxy resin may be selected from any one of bisphenol a type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, and aromatic heterocyclic type epoxy resin.
Generally, the metal in the two-dimensional sheet metal nano filler is selected according to the common general knowledge in the art and the conventional metal for heat conduction in the market, and an appropriate heat-conducting metal can be selected according to the actual use requirement and scene of the heat-conducting material. Generally speaking, the two-dimensional flaky metal nanofiller of the present invention may be selected from one or more of two-dimensional flaky metal nickel nanosheets, two-dimensional flaky metal aluminum nanosheets, two-dimensional flaky metal copper nanosheets, two-dimensional flaky metal silver nanosheets, two-dimensional flaky metal platinum nanosheets, and two-dimensional flaky metal iron nanosheets, and may also cover two-dimensional flaky alloy nanosheets including the above metals. The two-dimensional sheet metal nano-filler can be directly purchased products with the average sheet thickness and the average outer diameter defined by the invention, and can also be prepared by referring to the prior art.
Typically, the diluent is an organic solvent compatible with the epoxy resin, and those skilled in the art can select common general knowledge and commercially available organic reagents according to actual production conditions. In order to better illustrate the present invention and provide several preferred technical solutions for reference due to the requirement criteria of low toxicity and environmental protection in the industrial production process, the diluent is selected from one or more of ethanol, petroleum ether, isobutanol, hexane, n-hexane, cyclohexane and dichloromethane. It is worth to say that the effective dispersion of the two-dimensional flaky metal nano filler and the two-dimensional flaky carbon-based heat-conducting filler is realized by the adaptive addition of the diluent.
The two-dimensional sheet carbon-based heat-conducting filler is selected according to common knowledge in the art and conventional carbon-based fillers for heat conduction in the market, and an appropriate carbon-based filler can be selected according to actual use requirements and scenes of the heat-conducting material. Generally speaking, the two-dimensional flaky carbon-based heat conductive filler provided by the invention can be selected from one or more of two-dimensional flaky graphene, two-dimensional flaky microsilica flake, two-dimensional flaky nano-graphite flake and two-dimensional flaky expanded graphite. The two-dimensional flaky carbon-based heat-conducting filler can be directly purchased products with the average lamella thickness and the average outer diameter defined by the invention, and can also be prepared by referring to the prior art.
In addition to the two-dimensional flaky metal nanofiller and the two-dimensional flaky carbon-based heat conductive filler, other processing aids such as antioxidants, flame retardants, anti-aging agents and the like known in the prior art can be added. However, it is a prerequisite that these processing aids do not adversely affect the achievement of the objects of the present invention and the achievement of the advantageous effects of the present invention.
Furthermore, the invention also provides a preparation method of the epoxy two-dimensional flaky metal nano filler ultrahigh isotropic heat conduction material, and a prepared finished product can be an intermediate material of a heat conduction workpiece and can also be directly hot-pressed and molded into the heat conduction workpiece according to a mold.
A preparation method of an epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) according to parts by weight, 5-25 parts of epoxy resin, 60-90 parts of two-dimensional flaky metal nano filler, 5-15 parts of two-dimensional flaky carbon heat-conducting filler and 10-40 parts of diluent are compounded, and stirred and mixed under the condition that the stirring speed is 500-2000 r/min, so that a resin-filler compound with uniformly dispersed filler is obtained;
wherein the average lamella thickness of the two-dimensional flaky metal nano filler is 100-500 nm, the average outer diameter is 10-100 μm,
the average lamella thickness of the two-dimensional flaky carbon-based heat-conducting filler is 10-500 nm, and the average outer diameter is 1-50 mu m;
(2) placing the resin-filler compound obtained in the step (1) under the conditions of room temperature, normal pressure or room temperature and negative pressure, and ensuring the sufficient removal of the diluent after the diluent is completely volatilized;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, and carrying out hot-pressing curing for 1-5 hours at 100-190 ℃ and under 5-20 MPa to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional flaky metal nanofiller.
Generally, the stirring and mixing time in step (1) depends on the specific addition weight of each component in step (1), and one skilled in the art can observe that the black carbon-based filler is uniformly dispersed among the metal fillers and has no obvious black color lumps according to the actual addition amount. In order to better illustrate the present invention and provide a preferable technical solution for reference, the epoxy resin is stirred and mixed for more than 5min under laboratory conditions when the addition amount of the epoxy resin is less than 100 g. In the actual industrialization process, technicians can increase the stirring and mixing time according to the actual weight of the raw materials.
Wherein, the room temperature and negative pressure condition in the step (2) is selected by the conventional technology in the technical field for accelerating the volatilization of the diluent, and the person skilled in the art can select a proper negative pressure value according to the prior art. For better illustration of the invention and for reference, a preferred solution is provided, said room temperature negative pressure condition being preferably-0.5 to-1 MPa.
Wherein, the diluent to be diluted in the step (2) is completely volatilized, the specific volatilization time depends on the specific addition weight of each component in the step (1), and a person skilled in the art can adjust the volatilization time according to the actual addition amount, and the volatilization time is usually 1-24 hours.
Further, in the step (3), hot-press curing is carried out for 1-5 hours under the conditions of 100-190 ℃ and 5-20 MPa, the hot-press curing can be selectively divided into a plurality of stages, preferably 2-4 stages with different temperatures for hot-press curing, the temperature of the latter stage is 20-60 ℃ higher than that of the former stage, and the hot-press curing time of each stage is 1-3 hours.
Through tests, the thermal conductivity of the ultrahigh isotropic heat conduction material of the finally prepared epoxy group two-dimensional sheet metal nano filler reaches more than 10W/m.K, and the tensile strength is 25-45 MPa.
Further, to better illustrate the present invention and provide a preferred technical solution, on the premise of satisfying that the tensile strength is not reduced compared with pure epoxy-based resin, the thermal conductivity of the final ultra-high isotropic thermal conductive material of epoxy-based two-dimensional sheet metal nano-filler is improved as much as possible:
the preferable proportion of the two-dimensional flaky metal nano filler for heat conduction in the step (1) is 80-90 parts; the two-dimensional flaky carbon heat-conducting filler is preferably two-dimensional flaky graphene and two-dimensional flaky nanoscale graphite flakes, the total addition amount is 5-15 parts, and the mass ratio of the two-dimensional flaky carbon heat-conducting fillers is 1 (1-2);
the technological parameters of the hot-pressing solidification in the step (2) are as follows: the curing temperature is 120-180 ℃, and the pressure is 15-20 MPa.
According to the preferable technical scheme, the thermal conductivity of the ultrahigh isotropic heat conduction material of the prepared epoxy group two-dimensional sheet metal nano filler is 13-15W/m.K, and the tensile strength is 25-32 MPa.
Further, in order to better illustrate the present invention and provide a preferable technical solution, on the premise that the thermal conductivity is not lower than 10W/m · K, the mechanical properties of the final ultra-high isotropic thermal conductive material of the epoxy-based two-dimensional sheet metal nanofiller are improved as much as possible:
the preferable proportion of the two-dimensional flaky metal nano filler for heat conduction in the step (1) is 60-75 parts; the two-dimensional flaky carbon heat-conducting filler is preferably a micron-sized graphite sheet, and the addition amount is 5-8 parts;
the technological parameters of the hot-pressing solidification in the step (2) are as follows: the curing temperature is 120-180 ℃, and the pressure is 15-20 MPa.
According to the preferable technical scheme, the thermal conductivity of the ultrahigh isotropic heat conduction material of the prepared epoxy group two-dimensional sheet metal nano filler is not lower than 10W/m.K, and the tensile strength is 35-45 MPa.
It should be noted that the two-dimensional sheet metal nano-filler is a metal sheet with a nano-scale thickness prepared by grinding micron-sized metal particles. Has the characteristics of thin thickness, good flexibility, good dispersibility and high intrinsic thermal conductivity. Compared with metal nano particles, the metal nano sheet has the characteristics of low production cost and easiness in forming a heat conduction network. However, because the two-dimensional sheet metal nano-filler has a special lamellar structure and high rigidity, if the two-dimensional sheet metal nano-filler is filled with polymer-based materials such as epoxy resin and the like alone, sufficient overlapping between lamellae is difficult to realize, the improvement of the heat conductivity coefficient is very limited, and the high heat conduction requirement cannot be met. In the prior art, two-dimensional sheet metal nano-fillers are usually filled in a matrix material in an oriented manner, so that high thermal conductivity in plane or in certain orientation is obtained through combination and orientation of a special sheet structure, but the thermal conductivity in a non-oriented direction is usually very poor and cannot meet the thermal conductivity requirement, so that the thermal conductive materials usually have a plurality of limitations in material shapes (mostly thermal conductive films) and application.
The invention is characterized in that the inventor finds that the two-dimensional flaky metal nano filler and the non-traditional granular filler, especially the bendable flexible high-length-diameter ratio two-dimensional flaky carbon heat-conducting filler are compounded, so that the two-dimensional flaky carbon heat-conducting filler can be fully dispersed and overlapped between metal sheet layers, the heat conductivity in the direction vertical to the orientation direction of the metal sheet can be effectively improved, a more efficient isotropic heat-conducting path is constructed, and the efficient synergistic effect between the two-dimensional flaky metal nano filler and the non-spherical carbon filler is realized. Through a large number of tests and exploration, based on experimental facts, a form of compounding a two-dimensional flaky metal nano filler and a two-dimensional flaky carbon heat-conducting filler is determined, the two-dimensional flaky metal nano filler is used as a main heat-conducting filler, the two-dimensional flaky metal nano filler and a relatively small amount of the two-dimensional flaky carbon heat-conducting filler are added into epoxy resin together, the prepared heat-conducting material has the characteristic of isotropic heat conduction, the heat-conducting property is greatly improved, the heat-conducting coefficient is larger than 10W/m.K, and the preparation method has a very remarkable progress effect.
It is worth to be emphasized that the carbon-based heat-conducting filler is limited to a two-dimensional sheet-like carbon-based heat-conducting filler with a high length-diameter ratio, and because the carbon-based filler has good flexibility, the bending and folding of the filler between the two-dimensional sheet-like metal nano-fillers can be realized, and the adjacent metal sheet layers can be better connected to construct more heat-conducting paths. Based on the experimental facts, the specific specification parameters of the two-dimensional flaky carbon-based heat-conducting filler are determined through a control experiment: the two-dimensional sheet-like carbon-based heat conductive filler has an average sheet thickness of 10 to 500nm and an average outer diameter of 1 to 50 μm. If the traditional granular carbon-based filler is selected, the particles cannot realize sufficient filler lap joint between the two-dimensional flaky metal nano fillers due to the low length-diameter ratio, so that the heat conductivity perpendicular to the lamellar direction is not greatly improved; if the flaky carbon-based filler with the specification larger than the specification defined by the invention is selected, the flexibility and foldability of the filler are obviously reduced, the filler cannot form effective lap joint with the two-dimensional flaky metal nano filler and form an efficient heat conduction path, the filler gap is increased, and the heat conductivity and the mechanical property are reduced.
In addition, the two-dimensional flaky carbon-based heat-conducting filler is defined by fully considering that compared with other types of one-dimensional fillers, the two-dimensional flaky carbon-based heat-conducting filler has better flexibility and good bending folding performance, and can be well dispersed among the two-dimensional flaky metal nano fillers to form effective lap joint.
It is worth to be further noted that the addition amount of the two-dimensional flaky metal nano-filler is limited by a control experiment based on experimental facts, if the addition amount of the two-dimensional flaky metal nano-filler is less than 50 parts, although the heat conductivity of the system is still improved to a certain extent compared with that of a pure epoxy matrix, the improvement range is not large, because when the low-content metal filler is dispersed in the epoxy matrix, the interval between the sheet layers is large, and the added small amount of flaky carbon filler cannot form effective and dense lap joints between the metal nano-sheets, so that an effective heat conduction path cannot be formed; if the addition amount of the two-dimensional sheet metal nano filler is more than 95 parts, the epoxy resin ratio is easily too low, the bonding effect among the fillers is poor, the forming effect of the epoxy composite material is poor, a large amount of air thermal resistance is easily caused, and the mechanical property is greatly reduced.
It should be noted that the preparation method of the present invention is limited to the hot press forming process because the present invention is based on the above inventive principle. If the resin-filler composite with uniformly dispersed filler is prepared by a non-hot-press molding method, for example, the raw materials which are fully mixed are extruded and molded by an extruder, the thermal conductivity of the obtained sample is obviously lower than that of a hot-press curing molded sample. The reason is that the sample is in a normal pressure state after being extruded, the fillers in the sample cannot be in full contact, and the filler network has larger thermal resistance and lower thermal conductivity. The sample formed by hot-pressing solidification has the components contacted with each other under the action of pressure, and a high-efficiency heat transfer passage can be constructed, so that the hot-pressing solidification forming is the only known method capable of realizing the highest heat conductivity of the product.
The invention has the following beneficial effects:
1. according to the invention, two-dimensional flaky heat-conducting fillers are lapped in the epoxy resin matrix to form a three-dimensional heat-conducting network, so that the efficient lapping and efficient synergistic effect of the two-dimensional flaky metal nano-fillers are realized, the heat-conducting property of the obtained heat-conducting material or a product is greatly improved, and the three-dimensional flaky heat-conducting network has the characteristic of isotropic heat conduction.
2. The invention utilizes the special lamellar structure of the two-dimensional flaky metal nano filler and the high flexibility characteristic of the two-dimensional flaky carbon heat-conducting filler, combines the two, only needs the low addition amount of the two-dimensional flaky carbon heat-conducting filler, can realize the high-efficiency lap joint of the flaky metal filler, and has the characteristics of high-efficiency synergistic effect and isotropic heat conduction.
3. The heat conduction material or the product prepared by the invention has extremely high heat conduction performance, is greatly superior to the traditional single heat conduction metal filler heat conduction material system, and provides a new technical path for the subsequent compound heat conduction filler technical system.
4. The preparation method is simple, does not need special process equipment and processing conditions, is suitable for industrial implementation and transformation, and has good commercial application prospect.
Drawings
Fig. 1 is a photograph of a sample of the ultra-high isotropic thermal conductive material of the epoxy-based two-dimensional sheet metal nanofiller prepared in example 4 of the present invention.
Fig. 2 is a scanning electron microscope photograph of the ultrahigh isotropic thermal conductive material of the epoxy-based two-dimensional sheet metal nanofiller prepared in example 4 of the present invention. It can be obviously seen that the two-dimensional flaky carbon-based heat-conducting filler is tightly attached to the two-dimensional flaky metal nano-filler, and the orientation of the lamellar is not obvious.
Fig. 3 is a perspective electron microscope photograph of the ultra-high isotropic thermal conductive material of the epoxy-based two-dimensional sheet metal nanofiller prepared in example 4 of the present invention. It can be obviously seen that two-dimensional flaky carbon series heat-conducting fillers are uniformly distributed among the two-dimensional flaky metal nano fillers, and meanwhile, the two-dimensional flaky carbon series heat-conducting fillers are obviously contacted with the two-dimensional flaky metal nano fillers, so that establishment of a heat-conducting path is proved.
Fig. 4 is a photograph of a sample of the ultra-high isotropic thermal conductive material of the epoxy-based two-dimensional sheet metal nanofiller prepared in example 4 of the present invention when the thermal conductivity is measured. Type of thermal conductivity tester in the figure: hot Disk 2500-OT, Sweden, uses the Hot desk transient plane heat source method to test the thermal conductivity.
Fig. 5 is a detail photograph of ultra-high isotropic heat conduction material sample of epoxy-based two-dimensional sheet metal nano-filler prepared in example 4 of the present invention when testing heat conductivity.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings. It should be noted that the examples given are not to be construed as limiting the scope of the invention, and that those skilled in the art, on the basis of the teachings of the present invention, will be able to make numerous insubstantial modifications and adaptations of the invention without departing from its scope.
The following examples test criteria: the transient plane heat source method is based on ISO 22007-2-2008 standard to test Pyroceram9606 (reference document: [1] Wangqiang, Dajingmen, which tile, influence factor [ J ] of Tianjin university for measuring thermal conductivity based on Hot Disk method: Nature science and engineering technology edition, 2009(11):970-
Example 1
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is bisphenol A epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal iron nano sheet with the average lamella thickness of 100-300 nm and the average outer diameter of 10-15 mu m,
the two-dimensional flaky carbon-based heat-conducting filler is two-dimensional flaky graphene with the average lamellar thickness of 10-50 nm and the average outer diameter of 1-10 mu m,
the diluent is selected from petroleum ether.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing under the condition that the stirring speed is 1000r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under the condition of negative pressure of 1MPa, standing for 2 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, carrying out hot-pressing curing for 2 hours at 100 ℃ and 10MPa, then heating to 190 ℃, and carrying out hot-pressing curing for 2 hours under the same pressure to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nanofiller.
The ultra-high isotropic heat conduction material of the prepared epoxy-based two-dimensional sheet metal nano filler is used as a sample to be tested, the heat conductivity is 11W/m.K (anisotropic heat conductivity: the in-plane heat conductivity is 12W/m.K, the normal heat conductivity is 10.5W/m.K, and the material can be considered as an isotropic material), and the tensile strength is 37 MPa.
Example 2
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein, the epoxy resin is selected from aromatic heterocyclic epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal silver nano sheet with the average lamella thickness of 100-200 nm and the average outer diameter of 10-15 mu m,
the two-dimensional flaky carbon-based heat-conducting filler is a two-dimensional flaky micron graphite sheet with an average lamella thickness of 50-500 nm and an average outer diameter of 1-10 μm,
the diluent is ethanol.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing under the condition that the stirring speed is 800r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under the condition of negative pressure of 1MPa, standing for 4 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, carrying out hot-pressing curing at 120 ℃ and 18MPa for 2 hours, then heating to 150 ℃, carrying out hot-pressing curing at the same pressure for 2 hours, finally heating to 180 ℃, and curing under the same conditions for 1 hour to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nanofiller.
The ultra-high isotropic heat conduction material of the prepared epoxy-based two-dimensional sheet metal nano filler is used as a sample to be tested, the heat conductivity is 10W/m.K (anisotropic heat conductivity: in-plane heat conductivity is 10.7W/m.K, normal heat conductivity is 9.5W/m.K, and the material can be considered as an isotropic material), and the tensile strength is 35 MPa.
Example 3
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is bisphenol F type epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal aluminum nano sheet with the average lamella thickness of 100-200 nm and the average outer diameter of 10-20 mu m,
the two-dimensional flaky carbon-based heat-conducting filler is two-dimensional flaky expanded graphite with the average lamellar thickness of 50-500 nm and the average outer diameter of 1-10 μm,
the diluent is selected from n-hexane.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing at the stirring speed of 1500r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under a normal pressure condition, standing for 24 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, carrying out hot-pressing curing at 100 ℃ and 13MPa for 2 hours, then heating to 130 ℃, carrying out hot-pressing curing at the same pressure for 1 hour, finally heating to 190 ℃, and curing under the same conditions for 1 hour to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nanofiller.
The ultra-high isotropic heat conduction material of the prepared epoxy-based two-dimensional sheet metal nano filler is used as a sample to be tested, the heat conductivity is 13W/m.K (anisotropic heat conductivity: the in-plane heat conductivity is 14.0W/m.K, the normal heat conductivity is 12.4W/m.K, and the material can be considered as an isotropic material), and the tensile strength is 30 MPa.
Example 4
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is bisphenol F type epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal copper nano sheet with the average lamella thickness of 100-300 nm and the average outer diameter of 10-20 mu m,
the two-dimensional flaky carbon-based heat-conducting filler is a two-dimensional flaky nano graphite sheet with an average lamella thickness of 50-500 nm and an average outer diameter of 1-10 μm,
the diluent is selected from isobutanol.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing under the condition that the stirring speed is 2000r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under a normal pressure condition, standing for 18 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, carrying out hot-pressing curing at 120 ℃ and 20MPa for 3 hours, then heating to 180 ℃, and curing under the same condition for 1.5 hours to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nanofiller.
The ultra-high isotropic heat conduction material of the prepared epoxy-based two-dimensional sheet metal nano filler is used as a sample to be tested, the heat conductivity is 13.5W/m.K (anisotropic heat conductivity: the in-plane heat conductivity is 14.0W/m.K, the normal heat conductivity is 13W/m.K, and the material can be considered as an isotropic material), and the tensile strength is 28 MPa.
Example 5
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is selected from polyphenol type glycidyl ether epoxy resin,
the two-dimensional flaky metal nano-filler is a two-dimensional flaky metal platinum nano-sheet with the average lamella thickness of 100-200 nm and the average outer diameter of 10-20 mu m,
the two-dimensional flaky carbon-based heat-conducting filler is a two-dimensional flaky nano graphite sheet with an average lamella thickness of 50-500 nm and an average outer diameter of 1-10 μm,
the diluent is selected from cyclohexane.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing under the condition that the stirring speed is 1600r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under the condition of negative pressure of 0.5MPa, standing for 6 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, carrying out hot-pressing curing at 130 ℃ and 15MPa for 2 hours, then heating to 150 ℃, curing for 1 hour under the same condition, finally heating to 180 ℃, and curing for 1 hour under the same condition to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional flaky metal nanofiller.
The ultra-high isotropic heat conduction material of the prepared epoxy-based two-dimensional sheet metal nano filler is used as a sample to be tested, the heat conductivity is 15W/m.K (anisotropic heat conductivity: in-plane heat conductivity is 13.9W/m.K, normal heat conductivity is 15.5W/m.K, and the material can be considered as an isotropic material), and the tensile strength is 25 MPa.
Example 6
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is bisphenol A epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal nickel nano sheet with the average lamella thickness of 300-500 nm and the average outer diameter of 50-100 mu m,
the two-dimensional flaky carbon-based heat-conducting filler is two-dimensional flaky graphene with the average lamellar thickness of 200-500 nm and the average outer diameter of 30-50 μm,
the diluent is selected from hexane.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing under the condition that the stirring speed is 1000r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under a normal pressure condition, standing for 3 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, and carrying out hot-pressing curing for 3 hours at 100 ℃ and 15MPa to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler.
Example 7
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is bisphenol F type epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal copper nano sheet with the average lamella thickness of 100-400 nm and the average outer diameter of 20-100 mu m,
the two-dimensional flaky carbon heat-conducting filler is two-dimensional flaky graphene and two-dimensional flaky nanoscale graphite flakes with the average lamellar thickness of 100-500 nm and the average outer diameter of 10-50 mu m, and the mass ratio of the two-dimensional flaky carbon heat-conducting fillers is 1: 2;
the diluent is selected from petroleum ether.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing under the condition that the stirring speed is 2000r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under a normal pressure condition, standing for 12 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressurizing the resin-filler compound subjected to diluent removal in the step (2) by a press, and carrying out hot-pressing curing for 4 hours at 160 ℃ and 20MPa to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler.
Example 8
The ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler mainly comprises the following components in parts by weight:
wherein the epoxy resin is selected from aliphatic glycidyl ether epoxy resin,
the two-dimensional flaky metal nano filler is a two-dimensional flaky metal iron nanosheet and a two-dimensional flaky metal copper nanosheet which have the average lamella thickness of 200-500 nm and the average outer diameter of 50-100 mu m, and the mass ratio of the two-dimensional flaky metal nano fillers is 1: 1;
the two-dimensional flaky carbon-based heat-conducting filler is two-dimensional flaky graphene with the average lamellar thickness of 300-500 nm and the average outer diameter of 40-50 μm,
the diluent is dichloromethane.
The preparation method of the epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material mainly comprises the following steps:
(1) compounding epoxy resin, two-dimensional flaky metal nano filler, two-dimensional flaky carbon series heat conducting filler and diluent according to the proportion, and stirring and mixing at the stirring speed of 1500r/min to obtain a resin-filler compound with uniformly dispersed filler;
(2) placing the resin-filler compound obtained in the step (1) under a normal pressure condition, standing for 6 hours to enable the diluent to be completely volatilized, and ensuring the diluent to be fully removed;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, and carrying out hot-pressing curing for 4 hours at 180 ℃ and 5MPa to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional sheet metal nano filler.
Claims (10)
1. The ultrahigh isotropic heat conduction material of the epoxy two-dimensional flaky metal nano filler is characterized by mainly comprising the following components in parts by weight:
wherein the average lamella thickness of the two-dimensional flaky metal nano filler is 100-500 nm, the average outer diameter is 10-100 μm,
the average lamella thickness of the two-dimensional flaky carbon-based heat-conducting filler is 10-500 nm, and the average outer diameter is 1-50 μm.
2. The thermally conductive material of claim 1, wherein: the epoxy resin is selected from any one of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester epoxy resin and aromatic heterocyclic epoxy resin.
3. The thermally conductive material of claim 1, wherein: the two-dimensional flaky metal nano filler comprises any one or more of a two-dimensional flaky metal nickel nanosheet, a two-dimensional flaky metal aluminum nanosheet, a two-dimensional flaky metal copper nanosheet, a two-dimensional flaky metal silver nanosheet, a two-dimensional flaky metal platinum nanosheet and a two-dimensional flaky metal iron nanosheet, and can also cover a two-dimensional flaky alloy nanosheet comprising the metal.
4. The thermally conductive material of claim 1, wherein: the diluent is selected from one or more of ethanol, petroleum ether, isobutanol, hexane, n-hexane, cyclohexane and dichloromethane.
5. The thermally conductive material of claim 1, wherein: the two-dimensional flaky carbon-based heat-conducting filler is compounded by one or more of two-dimensional flaky graphene, two-dimensional flaky micron graphite flakes, two-dimensional flaky nano graphite flakes and two-dimensional flaky expanded graphite.
6. A preparation method of an epoxy two-dimensional sheet metal nano filler ultrahigh isotropic heat conduction material is characterized by mainly comprising the following steps:
(1) according to parts by weight, 5-25 parts of epoxy resin, 60-90 parts of two-dimensional flaky metal nano filler, 5-15 parts of two-dimensional flaky carbon heat-conducting filler and 10-40 parts of diluent are compounded, and stirred and mixed under the condition that the stirring speed is 500-2000 r/min, so that a resin-filler compound with uniformly dispersed filler is obtained;
wherein the average lamella thickness of the two-dimensional flaky metal nano filler is 100-500 nm, the average outer diameter is 10-100 μm,
the average lamella thickness of the two-dimensional flaky carbon-based heat-conducting filler is 10-500 nm, and the average outer diameter is 1-50 mu m;
(2) placing the resin-filler compound obtained in the step (1) under the conditions of room temperature, normal pressure or room temperature and negative pressure, and ensuring the sufficient removal of the diluent after the diluent is completely volatilized;
(3) and (3) pressing the resin-filler compound subjected to diluent removal in the step (2) by a press, and carrying out hot-pressing curing for 1-5 hours at 100-190 ℃ and under 5-20 MPa to obtain the ultrahigh isotropic heat conduction material of the epoxy two-dimensional flaky metal nanofiller.
7. The method according to claim 6, wherein: the room temperature negative pressure condition in the step (2) is-0.5 to-1 Mpa.
8. The method according to claim 6, wherein: in the step (3), hot-pressing curing is carried out for 1-5 hours under the conditions of 100-190 ℃ and 5-20 MPa, the hot-pressing curing is carried out in 2-4 stages with different temperatures, the temperature of the latter stage is 20-60 ℃ higher than that of the former stage, and the hot-pressing curing time of each stage is 1-3 hours.
9. The method according to claim 6, wherein:
the preferable proportion of the two-dimensional flaky metal nano filler for heat conduction in the step (1) is 80-90 parts; the two-dimensional flaky carbon heat-conducting filler is preferably two-dimensional flaky graphene and two-dimensional flaky nanoscale graphite flakes, the total addition amount is 5-15 parts, and the mass ratio of the two-dimensional flaky carbon heat-conducting fillers is 1 (1-2);
the technological parameters of the hot-pressing solidification in the step (2) are as follows: the curing temperature is 120-180 ℃, and the pressure is 15-20 MPa.
10. The method according to claim 6, wherein:
the preferable proportion of the two-dimensional flaky metal nano filler for heat conduction in the step (1) is 60-75 parts; the two-dimensional flaky carbon heat-conducting filler is preferably a micron-sized graphite sheet, and the addition amount is 5-8 parts;
the technological parameters of the hot-pressing solidification in the step (2) are as follows: the curing temperature is 120-180 ℃, and the pressure is 15-20 MPa.
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