CN114774856A - Preparation method of graphene heat-conducting film - Google Patents
Preparation method of graphene heat-conducting film Download PDFInfo
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- CN114774856A CN114774856A CN202210459705.4A CN202210459705A CN114774856A CN 114774856 A CN114774856 A CN 114774856A CN 202210459705 A CN202210459705 A CN 202210459705A CN 114774856 A CN114774856 A CN 114774856A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0005—Separation of the coating from the substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
Abstract
The invention relates to the field of film preparation methods, in particular to a preparation method of a graphene heat-conducting film. The method comprises the following steps: A. cleaning a nickel foil; B. putting a powdery solid carbon source into a crucible, horizontally placing a nickel foil at the opening of the crucible, horizontally pressing a high-temperature-resistant frame on the nickel foil, integrally inverting and putting into a furnace chamber to protect the atmosphere and heat at normal pressure, and controlling the growth temperature and the heat preservation time to grow a graphene thick film on the other surface of the nickel foil. Compared with two forming methods commonly used by graphene heat-conducting films, the method disclosed by the invention not only solves the problem that the graphene heat-conducting film with the thickness of 250nm-10um is not easy to form, has important significance for heat dissipation of microelectronic devices, but also does not need a high-temperature graphitization treatment process, and is short in production period, low in energy consumption and easy to expand.
Description
Technical Field
The invention relates to the field of film preparation methods, in particular to a preparation method of a graphene heat-conducting film.
Background
As electronic devices are moving to miniaturization and multi-functionalization, serious heat dissipation problems inevitably result. The requirement for thermal management materials to have ultra-high thermal conductivity, as well as ultra-thin and flexible properties to match complex and highly integrated power systems, the efficiency of heat dissipation has become a critical issue that determines the reliability and stability of the device components. The graphene film has important application potential as a thermal management material due to high flexibility and high thermal conductivity, and particularly can effectively diffuse locally generated heat in equipment with a complex structure.
At present, the graphene heat-conducting film is mainly formed by two modes: the method comprises the following steps of firstly, using a PI film as a precursor, carrying out carbonization and graphitization process treatment to obtain the graphene heat-conducting film, and secondly, using graphene oxide slurry as a precursor, and carrying out coating, drying, carbonization, graphitization and mould pressing to obtain the graphene heat-conducting film. However, the thickness of the heat-conducting film formed by the two modes is more than or equal to 10um, and with the increasing trend of miniaturization of electronic devices, higher requirements are also put forward on the thickness of the heat-conducting film, and the forming process is difficult to realize at present for the thickness range of 250nm-10 um.
Disclosure of Invention
The invention provides a preparation method of a graphene heat-conducting film, and aims to overcome the defect that the heat-conducting film with the thickness of 250nm-10 mu m is difficult to form in the prior art.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of a graphene heat conduction film comprises the following steps:
A. ultrasonically cleaning the nickel foil by using acetone and pure water in sequence, and then drying the nickel foil by using N2;
B. putting a powdery solid carbon source into a crucible, horizontally putting a nickel foil on a crucible opening, horizontally pressing a high-temperature-resistant frame on the nickel foil, integrally and inversely putting the nickel foil into a heating area of a quartz tube, installing flanges at two ends of the quartz tube, vacuumizing to 15-35 Pa, filling inert gas to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen to enable a furnace chamber to be in a normal pressure state, and simultaneously opening a heating system to heat;
C. cooling after the temperature of the furnace is raised to 1050-1200 ℃ and the temperature is kept for 0.5-8 h;
D. and taking out the nickel foil with the graphene growing on the surface, corroding the nickel foil with dilute hydrochloric acid, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film.
According to another embodiment of the invention, it is further comprised that the nickel foil has a thickness of 50-150 um.
According to another embodiment of the present invention, the thickness of the nickel foil is 100-150 um.
According to another embodiment of the invention, further comprising the solid carbon source occupies 40-90% of the crucible volume.
According to another embodiment of the invention, it further comprises that the solid carbon source occupies 70-90% of the crucible volume.
According to another embodiment of the present invention, it is further included that the solid carbon source is one of carbon black powder, graphene oxide powder, activated carbon powder, and petroleum coke powder.
According to another embodiment of the present invention, further comprising the dilute hydrochloric acid concentration is 1 mol/L.
According to another embodiment of the invention, the method further comprises a step C, wherein the furnace temperature is 1100-1150 ℃.
According to another embodiment of the present invention, further comprising the step C, the holding time is 1-5 hours.
According to another embodiment of the invention, the method further includes that in the step A, the thickness of the graphene heat conduction film is 250nm-10um, and the heat conduction system is not less than 2800w/m.
Compared with two forming methods commonly used for graphene heat-conducting films, the method disclosed by the invention not only solves the problem that the graphene heat-conducting film with the thickness of 250nm-10um is not easy to form, and has an important significance for heat dissipation of microelectronic devices, but also does not need a high-temperature graphitization treatment process, and is short in production period, low in energy consumption and easy to expand.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic view of the structure of a crucible and a frame of the present invention;
fig. 2 is a raman spectrum of a graphene film grown according to the present invention;
in the figure, 1 is a crucible, 2 is a solid carbon source, 3 is a nickel foil, and 4 is a frame.
Detailed Description
FIG. 1 is a schematic view of the structure of a crucible and a frame according to the present invention; fig. 2 is a raman spectrum of the grown graphene film of the present invention.
With reference to fig. 1 and fig. 2, a method for preparing a graphene thermal conductive film includes the steps of:
A. ultrasonically cleaning the nickel foil 3 by using acetone and pure water in sequence, and then drying by using N2;
B. putting a powdery solid carbon source 2 into a crucible 1, horizontally placing a nickel foil 3 at the opening of the crucible 1, horizontally pressing a high-temperature-resistant frame 4 on the nickel foil 3, integrally and inversely putting the nickel foil into a heating area of a quartz tube, mounting flanges at two ends of the quartz tube, vacuumizing to 15-35 Pa, filling inert gas to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen, enabling a furnace chamber to be in a normal pressure state, and simultaneously opening a heating system to heat;
C. cooling after the temperature of the furnace rises to 1050-1200 ℃ and the temperature is kept for 0.5-8 h;
D. and taking out the nickel foil 3 with the graphene growing on the surface, corroding the nickel foil 3 with dilute hydrochloric acid, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film.
The first embodiment is as follows:
A. ultrasonically cleaning the nickel foil 3 with the thickness of 120um by using acetone and pure water in sequence, and then drying by using N2;
B. putting powdered carbon black accounting for 75% of the volume of a crucible 1 into an alumina crucible 1, horizontally placing a nickel foil 3 on the opening of the alumina crucible 1, horizontally pressing an alumina frame 4 on the nickel foil 3, integrally and inversely placing the nickel foil 3 into a heating area of a quartz tube, installing flanges at two ends of the quartz tube, vacuumizing to 15Pa, filling nitrogen to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen with the flow of 5/0.2SLM to enable a furnace chamber to be in the normal pressure state, and simultaneously opening a heating system to heat;
C. after the furnace temperature rises to 1100 ℃, preserving the heat for 1 hour and then cooling;
D. and taking out the nickel foil 3 with the graphene growing on the surface, corroding the nickel foil 3 with a dilute hydrochloric acid solution with the concentration of 1mol/L, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film. As shown in the attached figure 2, the graphene thick film grown by the method has a characteristic signal of obvious graphitized structure, ID/IG<0.01, which shows that the graphene thick film grown by the method has good quality. The thickness of the graphene film grown by the method is 250nm, and the thermal conductivity coefficient of the graphene thermal conductive film grown by the method is 2800W/m.K through testing of a laser thermal conductivity tester.
The second embodiment:
A. ultrasonically cleaning a nickel foil 3 with the thickness of 125um by using acetone and pure water in sequence, and then drying by using N2;
B. putting powdered graphene oxide accounting for 70% of the volume of a crucible 1 into the silicon carbide crucible 1, horizontally placing a nickel foil 3 on the opening of the silicon carbide crucible 1, horizontally pressing a graphite frame 4 on the nickel foil 3, integrally and inversely placing the nickel foil 3 into a heating area of a quartz tube, installing flanges at two ends of the quartz tube, vacuumizing to 20Pa, filling nitrogen to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen with the flow of 5/0.2SLM to enable the furnace chamber to be in a normal pressure state, and simultaneously opening a heating system to heat;
C. cooling after the furnace temperature rises to 1120 ℃ and the temperature is preserved for 1.5 hours;
D. and taking out the nickel foil 3 with the graphene growing on the surface, corroding the nickel foil 3 with a dilute hydrochloric acid solution with the concentration of 1mol/L, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film. The thickness of the graphene film grown by the method is 300nm, and the thermal conductivity coefficient of the graphene thermal conductive film grown by the method is 2950W/m.K, which is obtained by testing with a laser thermal conductivity tester.
Example three:
A. ultrasonically cleaning nickel foil 3 with the thickness of 100um by using acetone and pure water in sequence, and then drying by using N2;
B. putting powdered activated carbon which accounts for 80% of the volume of a crucible 1 into an alumina crucible 1, horizontally placing a nickel foil 3 on the opening of the alumina crucible 1, horizontally pressing a quartz frame 4 on the nickel foil 3, integrally and inversely placing the nickel foil 3 into a heating area of a quartz tube, installing flanges at two ends of the quartz tube, vacuumizing to 25Pa, filling nitrogen to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen with the flow of 5/0.2SLM to enable a furnace chamber to be in a normal pressure state, and simultaneously opening a heating system to heat;
C. after the furnace temperature rises to 1150 ℃, preserving the heat for 5 hours and then cooling;
D. and taking out the nickel foil 3 with the graphene growing on the surface, corroding the nickel foil 3 with dilute hydrochloric acid with the concentration of 1mol/L, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film. The thickness of the graphene film grown by the method is 10 mu m, and the thermal conductivity coefficient of the graphene thermal conductive film grown by the method is 2250W/m.K through testing by a laser thermal conductivity tester.
Example four:
A. ultrasonically cleaning a nickel foil 3 with the thickness of 150um by using acetone and pure water in sequence, and then drying by using N2;
B. putting petroleum coke powder which accounts for 90 percent of the volume of a crucible 1 into a graphite crucible 1, horizontally placing a nickel foil 3 at the opening of the graphite crucible 1, horizontally pressing a graphite frame 4 on the nickel foil 3, integrally and inversely placing the graphite foil 3 into a heating area of a quartz tube, installing flanges at two ends of the quartz tube, vacuumizing to 30Pa, then filling nitrogen to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen with the flow of 5/0.2SLM (selected from the group consisting of Lash gas, Frost gas, Frost gas, Frost gas, Frost gas, Frost gas, Fr;
C. when the furnace temperature rises to 1135 ℃, preserving the heat for 3 hours and then cooling;
D. and taking out the nickel foil 3 with the graphene growing on the surface, corroding the nickel foil 3 with a dilute hydrochloric acid solution with the concentration of 1mol/L, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film. The thickness of the graphene film grown by the method is 5um, and the thermal conductivity coefficient of the graphene thermal conductive film grown by the method is 2450W/m.K through testing of a laser thermal conductivity tester.
Claims (10)
1. A preparation method of a graphene heat-conducting film is characterized by comprising the following steps:
A. ultrasonically cleaning the nickel foil (3) by using acetone and pure water in sequence, and then drying by using N2;
B. putting a powdery solid carbon source (2) into a crucible (1), horizontally putting a nickel foil (3) at the opening of the crucible (1), horizontally pressing a high-temperature-resistant frame (4) on the nickel foil (3), integrally and inversely putting the nickel foil into a heating area of a quartz tube, installing flanges at two ends of the quartz tube, vacuumizing to 15-35 Pa, filling inert gas to normal pressure, repeating the operation twice, opening an exhaust valve, continuously introducing mixed gas of nitrogen and hydrogen to enable a furnace chamber to be in a normal pressure state, and simultaneously opening a heating system to heat;
C. cooling after the temperature of the furnace rises to 1050-1200 ℃ and the temperature is kept for 0.5-8 h;
D. and taking out the nickel foil (3) with the graphene growing on the surface, corroding the nickel foil (3) with dilute hydrochloric acid, then cleaning the graphene film with pure water, and airing to obtain the graphene heat-conducting film.
2. The method for preparing the graphene thermal conductive film according to claim 1, wherein the thickness of the nickel foil (3) is 50-150 um.
3. The preparation method of the graphene thermal conductive film according to claim 2, wherein the thickness of the nickel foil (3) is 100-150 um.
4. The method for preparing the graphene thermal conductive film according to claim 1, wherein the solid carbon source (2) occupies 40-90% of the volume of the crucible (1).
5. The method for preparing the graphene thermal conductive film according to claim 4, wherein the solid carbon source (2) occupies 70-90% of the volume of the crucible (1).
6. The preparation method of the graphene thermal conductive film according to claim 1, wherein the solid carbon source (2) is one of carbon black powder, graphene oxide powder, activated carbon powder and petroleum coke powder.
7. The method for preparing the graphene thermal conductive film according to claim 1, wherein the concentration of the dilute hydrochloric acid is 1 mol/L.
8. The method for preparing the graphene thermal conductive film according to claim 1, wherein in the step C, the furnace temperature is 1100-1150 ℃.
9. The method for preparing a graphene thermal conductive film according to claim 1, wherein in the step C, the heat preservation time is 1-5 hours.
10. The preparation method of the graphene thermal conductive film according to claim 1, wherein the graphene thermal conductive film has a thickness of 250nm-10um, and a thermal conductive system of not less than 2800 w/m.K.
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