CN116003148A - High-thermal-conductivity graphene composite film and preparation method thereof - Google Patents
High-thermal-conductivity graphene composite film and preparation method thereof Download PDFInfo
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- CN116003148A CN116003148A CN202211590324.6A CN202211590324A CN116003148A CN 116003148 A CN116003148 A CN 116003148A CN 202211590324 A CN202211590324 A CN 202211590324A CN 116003148 A CN116003148 A CN 116003148A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 35
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 35
- 239000004964 aerogel Substances 0.000 claims abstract description 28
- 239000000017 hydrogel Substances 0.000 claims abstract description 25
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000007731 hot pressing Methods 0.000 claims abstract description 16
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 11
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 61
- 239000000463 material Substances 0.000 description 13
- 230000007547 defect Effects 0.000 description 8
- 238000005087 graphitization Methods 0.000 description 6
- 230000008439 repair process Effects 0.000 description 6
- 230000017525 heat dissipation Effects 0.000 description 5
- 239000004966 Carbon aerogel Substances 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
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- 239000002002 slurry Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 238000003825 pressing Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the field of microelectronics, and provides a high-heat-conductivity graphene composite film and a preparation method thereof, wherein the preparation method comprises the following steps: uniformly mixing graphene oxide and carbon nanotubes in a solvent, and performing hydrothermal reaction under a sealing condition to obtain hydrogel; freeze-drying the hydrogel to obtain aerogel; performing hot pressing on the aerogel to form a film; and (5) annealing and heat-treating the film to obtain the film. The method can effectively improve the dispersion of the carbon nano tube with low cost, and the hydrothermal reaction forms a three-dimensional graphene and carbon nano tube cross-linked structure. The aerogel is changed into a film sample through hot pressing, and the film sample prepared by the method still maintains good mechanical properties after heat treatment. The thickness of the prepared film varies from a few micrometers to hundreds of micrometers, and is an effective method for preparing thick films. Through experimental analysis, the electrical conductivity and the thermal conductivity can be effectively improved to be far higher than those of the composite film prepared by the common method.
Description
Technical Field
The invention belongs to the field of microelectronics, and particularly relates to a high-heat-conductivity graphene composite film and a preparation method thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
The development of portable devices and high power electronics creates serious heat dissipation problems that severely reduce the reliability and lifetime of the electronic device. High power devices are highly required to efficiently dissipate heat to maintain stable operation, and because of the rough surface of the thin film material, the space between the chip and the heat sink is filled with air, and the thermal conductivity of air (0.023W (mK) -1 ) Very low. Therefore, it is necessary to fill the thermal interface material to fill the microscopic gaps to improve the heat dissipation efficiency. To achieve this, thermal interface materials require excellent flexibility in addition to high thermal conductivity to match the roughness of the surface material to reduce contact resistance. In the 5G age, the need for thermal management by numerous devices has become more prominent. However, conventional thermal interface materials are inadequate to meet today's device requirements, and there is a great need to find new thermal interface materials for integrated circuits and devices to enhance heat dissipation.
The graphene heat-conducting film is usually prepared by solution suction filtration, coating, chemical vapor deposition and the like. These methods are all cost-effective methods for preparing graphene films. Graphene oxide contains abundant functional groups, is easy to disperse in water, is reduced into graphene at a higher temperature, and then is subjected to graphitization to repair lattice defects, so that the performance of the graphene is improved. However, due to the characteristics of the graphene material, the graphene is connected by only weak van der waals force between layers, so that the graphene is easy to slip and the out-of-plane thermal conductivity is not high. In order to improve the performance of graphene, a heat conducting filler is often introduced to enhance the heat conductivity of graphene. The most commonly used heat conducting filler is carbon nanotubes, however, the carbon nanotubes are extremely easy to aggregate and agglomerate, so that the performance of the material cannot reach the expected effect and even can be deteriorated, and therefore, the realization of effective dispersion of the carbon nanotubes becomes important.
The method for realizing the effective arrangement of the carbon nano tubes comprises the following steps: the CVD grows the carbon nano tube, realizes the effective arrangement of the carbon nano tube by using a strong electric field or a strong magnetic field, and the like, and has high requirement on realizing the dispersion of the carbon nano tube, complicated process or high cost. Therefore, the realization of effective dispersion of the carbon nanotubes and crosslinking with graphene is important for preparing the thermal interface material.
Patent 201710582990.8 discloses a preparation method of a copper foil-graphene/carbon nanotube or copper foil-graphene/carbon nanotube-copper foil heat conduction film, which is prepared by ball milling hydrogel after hydrothermal reaction into slurry and coating the slurry on a copper foil, but the mechanical properties of a sample prepared by the method are limited because the ball milling process can seriously damage the graphene carbon nanotube structure and related crosslinking, so that the mechanical properties of the coated sample are poor. The slurry of the method is influenced by factors such as tension, temperature and the like after being coated, and the sample has good flexibility.
Patent 202210644638.3 discloses a super-flexible multifunctional carbon aerogel and a preparation method thereof, but the preparation of the super-flexible multifunctional carbon aerogel is that the carbon aerogel is unfavorable for heat conduction due to larger porosity, which severely limits the application of the super-flexible multifunctional carbon aerogel as a thermal interface material.
Disclosure of Invention
In order to solve the problems, the invention provides a high-heat-conductivity graphene composite film and a preparation method thereof. The uniform dispersion of the carbon nanotubes can be effectively realized through hydrothermal reaction, a three-dimensional structure of the graphene sheets and the carbon nanotubes which are mutually crosslinked is formed, and the freeze-dried graphene-carbon nanotube aerogel is pressed into a film by applying external force, so that the method is a brand-new method for preparing the high-heat-conductivity film. The prepared film has better performance than the film prepared by the traditional method, has good flexibility, can effectively repair the defects of graphene after subsequent high-temperature heat treatment, and improves the electrical conductivity and the thermal conductivity of the film. The invention relates to a method for economically and effectively preparing a high-heat-conductivity graphene composite film, and the prepared film has excellent performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a preparation method of a high-heat-conductivity graphene composite film, which comprises the following steps:
uniformly mixing graphene oxide and carbon nanotubes in a solvent, and performing hydrothermal reaction under a sealing condition to obtain hydrogel;
freeze-drying the hydrogel to obtain aerogel;
performing hot pressing on the aerogel to form a film;
and (5) annealing and heat-treating the film to obtain the film.
According to the preparation method, graphene carbon nanotube hydrogel is prepared through hydrothermal reaction, aerogel is obtained through freeze drying, and then a film is formed through hot pressing. The method can prepare the film with controllable area and thickness, is suitable for industrial production, and can produce large-size high-heat-conductivity film. Thermal interface materials are generally required to have excellent thermal conductivity to increase their heat dissipation capability and good flexibility to reduce contact resistance.
In a second aspect of the invention, a high thermal conductivity graphene composite film prepared by the method is provided.
The aerogel is creatively pressed into the film through hot pressing, and the film sample with high heat conductivity is obtained through subsequent heat treatment. First, the distribution of the carbon nanotubes can be improved by a hydrothermal reaction, and crosslinks are formed between the carbon nanotubes and the graphene sheets. And then, the sample can basically keep a graphene carbon nano tube crosslinked structure formed by the hydrothermal reaction through freeze drying, so that the structural integrity of the sample is ensured. The heat pressing treatment can effectively reduce the porosity of the sample, improve the density of the film sample, change the sample from thicker aerogel to thinner film, and the change is critical to heat management, so that the heat dissipation capacity of the sample can be effectively improved. Since the film sample is obtained by pressing from aerogel, it has excellent flexibility and mechanical properties, which is helpful for the application of the sample as a thermal interface material. The higher the heat treatment temperature is, the more beneficial the heat conductivity is to be improved, the oxygen-containing functional groups are removed by heat treatment at the temperature higher than 2500 ℃, the lattice defects are repaired, and the electric conductivity and the heat conductivity are improved. Experiments show that the film sample prepared based on the method has the highest electric conductivity of 4300S/cm and the heat conductivity of 2000W (mK) -1 . In addition, the area and thickness of the film prepared by the method are controllable.
In a third aspect, the present invention provides an application of the graphene composite film with high thermal conductivity in manufacturing a portable device or a high-power electronic product.
The method provided by the invention is simple, the steps are easy to operate, and the high-heat-conductivity graphene composite film with excellent properties can be prepared at low cost, so that a new method and thinking are provided for practical thermal management.
The beneficial effects of the invention are that
(1) The invention relates to a graphene composite film based on hydrothermal reaction and a preparation method thereof, and the film prepared by the method has controllable sample area and thickness, the area is determined by the size of a reaction container, the thickness is 2um-200um, the electrical conductivity can 4300S/cm, and the thermal conductivity can reach 2000W (m K) -1 . The invention is a method for effectively preparing the graphene composite film material with low cost, and the film prepared based on the method has excellent mechanical properties, thereby providing a new method and thinking for practical thermal management.
(2) The invention is an effective method for preparing the graphite composite film, which can effectively improve the dispersion of the carbon nano tube with low cost and form a three-dimensional graphene and carbon nano tube cross-linking structure through hydrothermal reaction. The aerogel is changed into a film sample through hot pressing, and the film sample prepared by the method still maintains good mechanical properties after heat treatment. Through experimental analysis, the electrical conductivity and the thermal conductivity can be effectively improved to be far higher than those of the composite film prepared by the common method.
(3) The preparation method is simple, has strong practicability and is easy to popularize.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
Fig. 1: the preparation process of the invention is a flow chart.
Fig. 2: mechanical properties of the film samples prepared in example 1 of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The preparation method of the graphene composite film comprises the following steps:
mixing graphene oxide with a certain concentration and carbon nanotubes according to a certain mass ratio. The dispersion liquid is fully mixed and stirred and is placed in a reaction kettle. And placing the reaction kettle in a high-temperature furnace for hydrothermal reaction. Taking out the hydrogel formed by the high-temperature hydrothermal reaction, putting the hydrogel into a freeze dryer for freezing, and vacuumizing and drying the frozen hydrogel. And performing hot pressing treatment on the aerogel formed after freeze drying to change the aerogel into a film. And taking out the pressed film to perform heat treatment, and performing high-temperature heat treatment to further reduce graphene oxide and repair defects to obtain the high-heat-conductivity graphene composite film.
In some embodiments, the concentration of graphene oxide and carbon nanotubes is 1mg/ml to 5mg/ml, and the carbon nanotubes carry dangling bond hydroxyl groups. The formed hydrogel can be easily taken out and is not broken in the taking-out process only when the mass ratio of the graphene oxide to the carbon nano tube is more than or equal to 1.
In some embodiments, the graphene oxide to carbon nanotube mass ratio is 0.5-10.
In some embodiments, a total of greater than 30ml of the graphene oxide and carbon nanotube mixed dispersion is placed in a 500ml reaction kettle.
In some embodiments, the tightness of the reaction kettle is ensured, the hydrothermal reaction condition is 150-220 ℃, and the reaction time is 10-24 h.
In some embodiments, the hydrogel formed in the hydrothermal reaction kettle is removed and the hydrogel is placed in a freeze dryer and frozen for 12-24 hours.
In some embodiments, the frozen hydrogel is vacuum dried, and when the temperature of the aerogel is detected to be equal to ambient temperature, the drying is completed.
In some embodiments, the freeze-dried aerogel is removed, and the aerogel film is placed in a hot press for hot pressing at a pressure of 10MPa to 300MPa and a temperature of 30 ℃ to 150 ℃ for 1h to 24h.
In some embodiments, the film pressed by the hot press is removed and heat treated. The heat treatment comprises the annealing treatment under the protection of inert gas, wherein the annealing temperature is 300-1000 ℃, the heating rate is 0.2-5 ℃/min, and the annealing time is 1-10 h. The heat treatment also comprises graphitization treatment at the temperature of more than 2500 ℃, the graphitization temperature is 2500-3000 ℃, the defects of the film are repaired, and the performance of the film is improved.
The invention will now be described in further detail with reference to the following specific examples, which should be construed as illustrative rather than limiting.
In the following examples, graphene oxide was prepared by a modified Hummer method, and the carbon nanotubes were carboxylated multi-walled carbon nanotubes (purity >95%, outer diameter 8-15nm, length 50 um).
Example 1
The preparation method of the graphene composite film comprises the following steps:
and mixing graphene oxide and carbon nanotubes with the concentration of 2mg/ml according to the mass ratio of 1:1 or more. 30ml of the above dispersion was thoroughly mixed and stirred, and placed in a 500ml reaction vessel. The reaction vessel was placed in a high temperature furnace and subjected to hydrothermal reaction (high temperature 180 ℃ C., 12 h). Taking out the hydrogel formed by the high-temperature hydrothermal reaction, putting the hydrogel into a freeze dryer for freezing for 12 hours, vacuumizing and drying the frozen hydrogel, and finishing the drying when the temperature of the aerogel is detected to be equal to the ambient temperature. And (3) carrying out hot pressing treatment on the aerogel formed after freeze drying by a hot press (the pressure is 70MPa, the temperature is 70 ℃ and the time is 6 h), and carrying out hot pressing on the aerogel to obtain a film. And taking out the pressed film, placing the film in a tube furnace under the atmosphere of hydrogen-argon mixture, heating to 700 ℃ at a heating rate of 1 ℃/min, maintaining at 700 ℃ for 5 hours, and performing graphitization treatment at 2500 ℃ to reduce graphene through heat treatment to repair the defect.
The performance of the above films was tested: the thickness was determined by a 50-fold light microscope and software analysis. Conductivity was measured by the four terminal method and current and measurement voltage were provided by Keithley 2400. Thermal conductivityThe thermal diffusivity is measured by a laser flash method, and then according to the formula K=alpha×C P X ρ, K is the thermal conductivity, α is the thermal diffusivity, C P Is specific heat capacity and ρ is density.
The experimental test shows that: the prepared film sample has a thickness of about 15um, an electrical conductivity of up to about 4300S/cm, and a thermal conductivity of about 2000W (mK) -1 The mechanical properties of the film samples before and after heat treatment at 700 ℃ are shown in fig. 2 below.
Example 2
The preparation method of the graphene composite film comprises the following steps:
graphene oxide and carbon nanotubes with the concentration of 2.5mg/ml are mixed according to the mass ratio of 1:1.5 or more. 30ml of the above dispersion was thoroughly mixed and stirred, and placed in a 500ml reaction vessel. The reaction vessel was placed in a high temperature furnace and subjected to hydrothermal reaction (high temperature 190 ℃ C., 10 h). Taking out the hydrogel formed by the high-temperature hydrothermal reaction, putting the hydrogel into a freeze dryer for freezing for 12 hours, vacuumizing and drying the frozen hydrogel, and finishing the drying when the temperature of the aerogel is detected to be equal to the ambient temperature. And (3) carrying out hot pressing treatment on the aerogel formed after freeze drying by a hot press (the pressure is 80MPa, the temperature is 80 ℃ and the time is 4 hours), and carrying out hot pressing on the aerogel to obtain a film. Taking out the pressed film, placing the film in a tube furnace under the atmosphere of hydrogen-argon mixture, heating to 800 ℃ at a heating rate of 1 ℃/min, maintaining at 800 ℃ for 4 hours, and performing graphitization treatment at 2700 ℃ to reduce graphene by heat treatment to repair defects.
Example 3
The preparation method of the graphene composite film comprises the following steps:
graphene oxide and carbon nanotubes with the concentration of 2.2mg/ml are mixed according to the mass ratio of 1.5:1 or more. 30ml of the above dispersion was thoroughly mixed and stirred, and placed in a 500ml reaction vessel. The reaction vessel was placed in a high temperature furnace and subjected to hydrothermal reaction (high temperature 185 ℃ C., 11 h). Taking out the hydrogel formed by the high-temperature hydrothermal reaction, putting the hydrogel into a freeze dryer for freezing for 12 hours, vacuumizing and drying the frozen hydrogel, and finishing the drying when the temperature of the aerogel is detected to be equal to the ambient temperature. And (3) carrying out hot pressing treatment on the aerogel formed after freeze drying by a hot press (the pressure is 75MPa, the temperature is 75 ℃ and the time is 5 h), and carrying out hot pressing on the aerogel to obtain a film. The pressed film is taken out and placed in a tube furnace under the atmosphere of hydrogen-argon mixture gas, heated to 1000 ℃ at a heating rate of 1 ℃/min, and maintained at 1000 ℃ for 5.5 hours. And carrying out graphitization treatment at 2800 ℃ to reduce the graphene by heat treatment to repair the defect.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-heat-conductivity graphene composite film is characterized by comprising the following steps of:
uniformly mixing graphene oxide and carbon nanotubes in a solvent, and performing hydrothermal reaction under a sealing condition to obtain hydrogel;
freeze-drying the hydrogel to obtain aerogel;
performing hot pressing on the aerogel to form a film;
and (5) annealing and heat-treating the film to obtain the film.
2. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the concentration of graphene oxide and carbon nanotubes is 1-5 mg/ml.
3. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the hydrothermal reaction condition is 150-220 ℃ for 10-24 hours.
4. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the frozen hydrogel is dried by vacuum pumping, and when the temperature of the aerogel is detected to be equal to the ambient temperature, the drying is completed.
5. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the pressure of the hot pressing treatment is 10-300 MPa, the temperature is 30-150 ℃ and the time is 1-24 h.
6. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the annealing treatment temperature is 300-1000 ℃.
7. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the temperature of the heat treatment is 2500-3000 ℃.
8. The method for preparing a high thermal conductivity graphene composite film according to claim 1, wherein the mass ratio of graphene oxide to carbon nanotubes is 0.5-10.
9. The high thermal conductivity graphene composite film prepared by the method of any one of claims 1-8, wherein the film sample thickness is 2-200 um.
10. Use of the high thermal conductivity graphene composite film of claim 9 in the manufacture of portable devices or high power electronics.
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