CN111470490A - Oriented carbon nanotube/graphene composite heat-conducting film, preparation method thereof and semiconductor device - Google Patents
Oriented carbon nanotube/graphene composite heat-conducting film, preparation method thereof and semiconductor device Download PDFInfo
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Abstract
The invention discloses an oriented carbon nanotube/graphene composite heat-conducting film, a preparation method thereof and a semiconductor device.
Description
Technical Field
The invention belongs to the technical field of electronic devices, and particularly relates to an oriented carbon nanotube/graphene composite heat-conducting film, a preparation method thereof and a semiconductor device.
Background
With the wide use of electronic products and the integration of electronic devices, the development of the industries such as electronics and electricity tends to be more intensive and miniaturized, the devices release a large amount of heat during operation, and the problem of heat dissipation of electronic components is increasingly prominent. In the using process, the temperature of the working environment of the electric appliance can be increased rapidly due to poor heat conduction, so that the operation stability of electronic devices is influenced, and even the devices are damaged. Thermal Interface Materials (TIMs) play an important role between heat dissipation devices in order to allow for the timely conduction and removal of heat. In recent years, a large number of research reports indicate that carbon materials such as graphene, carbon graphite, carbon tubes and carbon fibers all have high thermal conductivity. Graphene (Graphene) has a hexagonal honeycomb structure formed by hybridizing carbon atoms based on sp2, and is only one atomic layer thick, so that the Graphene has excellent performances in many aspects such as heat, electricity and the like due to a special two-dimensional layered structure. Under room temperature conditions, the theoretical thermal conductivity of the graphene of the single layer can reach 5300W/(m · k), and the high thermal performance of the carbon (graphite) material mainly comes from the firm bonding among carbon atoms and the highly ordered lattice arrangement structure, so that the carbon (graphite) material is more and more emphasized in the preparation of high-performance TIM.
At present, patent documents (CN101597418, CN106185904, and CN106832758) for carbon-based graphene or carbon nanotube composite film preparation and thermal conductivity thereof mainly provide, for example, acidification treatment of carbon nanotubes to connect carboxyl groups on the carbon nanotubes, so as to improve carbon tube dispersibility, and can be uniformly dispersed in a polymer as a filler. The graphene oxide film generates folds in the hydriodic acid or ascorbic acid solution phase reduction process, so that pores appear in the carbon film, or the overlapping between the sheets is not proper in the film forming process of preparing and reducing the graphene oxide. In the preparation technology of the carbon nanotube and graphene heat-conducting film, simple mixing is usually adopted, so that the defect degree between the carbon tube and graphene sheets is high in the film forming process, the carbon tube and the graphene are in disordered overlapping, the phonon scattering is serious, and the heat-conducting performance of the carbon-based film is greatly limited.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide an aligned carbon nanotube/graphene composite thermal conductive film, a method for preparing the same, and a semiconductor device, so as to overcome the defects of the prior art, such as high defect degree between sheets, disordered overlapping, and serious phonon scattering in the thermal conduction process of a carbon tube and graphene in the film formation process.
The invention provides an oriented carbon nanotube/graphene composite heat-conducting film, which comprises a carbon nanotube layer and a graphene layer compounded on the surface of the carbon nanotube layer,
the carbon nanotube layer is an oriented film.
Preferably, in the oriented carbon nanotube/graphene composite thermal conductive film, the carbon nanotube layer is formed by interweaving carbon nanotube wires into a net shape.
Preferably, in the oriented carbon nanotube/graphene composite heat conductive film, graphene layers are compounded on both surfaces of the carbon nanotube layer.
In one embodiment of the invention, a semiconductor device is provided, and the oriented carbon nanotube/graphene composite heat conduction film is used as a heat conduction interface material.
An embodiment of the present invention provides a method for preparing an oriented carbon nanotube/graphene composite thermal conductive film, including:
s1, drawing the spinnable carbon nanotube array into an oriented film;
s2, compounding the graphene oxide solution on the surface of the orientation film;
and s3, carrying out heat treatment to obtain the composite heat conducting film.
Preferably, in the above method for preparing an oriented carbon nanotube/graphene composite thermal conductive film, in step s1, the spinnable carbon nanotube array is prepared by a chemical vapor deposition method.
Preferably, in the preparation method of the oriented carbon nanotube/graphene composite heat-conducting film, the growth temperature is 700-.
Preferably, in the above preparation method of the oriented carbon nanotube/graphene composite thermal conductive film, in step s2, the graphene oxide solution is compounded on the surface of the oriented film in a vacuum filtration, spraying, screen printing, inkjet printing, roll coating or knife coating manner.
Preferably, in the above method for preparing an oriented carbon nanotube/graphene composite thermal conductive film, in step s2, the concentration of the graphene oxide solution is 1-10mg/m L.
Preferably, in the above method for preparing an oriented carbon nanotube/graphene composite thermal conductive film, in step s3, the heat treatment process includes:
pretreating at 800-;
heating to 1500 and 2850 ℃ for high-temperature treatment for 0.5-2 hours.
According to the invention, carbon nanotubes are taken as a precursor, the carbon nanotubes are assembled into an ordered thin film structure by a film forming method, a graphene oxide solution with a certain concentration is compounded on the surface of the thin film in the film forming process to obtain an oriented carbon nanotube/graphene oxide composite thin film, and the obtained composite thin film is subjected to a high-temperature graphitization mode to prepare the one-dimensional and two-dimensional carbon nanomaterial composite heat-conducting film with high crystallinity and low defect.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of a carbon nanotube/graphene composite thermal conductive film according to an embodiment of the present invention;
fig. 2 is a schematic structural view of a carbon nanotube/graphene composite thermal conductive film according to another embodiment of the present invention;
FIG. 3a is a photograph showing a carbon nanotube layer according to an embodiment of the present invention;
FIG. 3b is a photograph showing a carbon nanotube layer according to another embodiment of the present invention;
fig. 4a shows an XRD pattern of the carbon tube/graphene composite film after high temperature treatment in example 1;
fig. 4b shows a Raman chart of the carbon tube/graphene composite film after high temperature treatment in example 1;
fig. 4c is a graph showing the in-plane thermal diffusion coefficient of the carbon tube/graphene composite film of example 1 after different high temperature treatments.
Detailed Description
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
Referring to fig. 1, an embodiment of the present invention provides a carbon nanotube/graphene composite thermal conductive film 10, including a carbon nanotube layer 11 and a graphene layer 12 compounded on a surface of the carbon nanotube 11, where the carbon nanotube layer 11 is an oriented film.
Referring to fig. 3a, the oriented carbon nanotube layer 11 may be extended in the same direction by carbon nanotube wires, and referring to fig. 3b, the oriented carbon nanotube layer 11 may also be woven into a net shape by carbon nanotube wires.
The thickness of the carbon nanotube layer 11 is preferably 80 to 300 nm.
Referring to fig. 2, in another embodiment, the carbon nanotube/graphene composite thermal conductive film 20 includes a carbon nanotube layer 21, and graphene layers 22 are laminated on two opposite surfaces of the carbon nanotube layer, so as to form a "sandwich" type composite film.
In other embodiments, the oriented carbon nanotube layers and graphene layers may be interleaved to form a stacked structure.
In the present case, carbon nanotube layer 11 need not add polyurethane polymer in the complex film to keep its pliability owing to adopt orientation film.
The obtained carbon nanotube/graphene composite heat-conducting film can be used as a heat-conducting interface material for microelectronics, communication, aerospace, military equipment, electric machines and electric appliances, such as L ED, and intelligent terminal products such as mobile phones and computers.
The embodiment of the invention also provides a preparation method of the carbon nanotube/graphene composite heat-conducting film, which comprises the following steps:
s1, adopting chemical vapor deposition method to grow the spinnable carbon nanotube array in the horizontal tube furnace in a controllable way, the carbon nanotube is made into the oriented self-supporting carbon tube film directly by the drawing way without dispersing or removing the growth substrate material.
(1) And placing the silicon wafer with the evaporated catalyst in a horizontal tube furnace, and then introducing inert gas to remove air in the furnace. And then, the furnace is heated according to a certain heating rate, the hydrogen and ethylene gas controller is opened at the same time, the temperature is raised to 750 ℃, the temperature is maintained for a period of time, and the sample of the spinnable carbon nanotube array is taken out after the temperature is reduced to room temperature.
In one embodiment, the catalyst is a nano-particle of a carbon-philic transition metal, such as iron, nickel, magnesium, molybdenum, and the like.
In one embodiment, the carbon source can also be acetylene.
In one embodiment, the inert gas in the furnace may be argon or nitrogen, with the exception of air.
In one embodiment, the temperature rise rate of the furnace is adjusted to 10-30 ℃/min.
In one embodiment, the growth heat preservation temperature can be adjusted to 700-840 ℃;
in one embodiment, the growth incubation time may be 10-60 min.
(2) The spinnable carbon nanotube array is drawn into carbon nanotube film by means of drawing technology.
In one embodiment, the film is drawn by a surgical knife or flat metal forceps.
In one embodiment, when the carbon nanotube film is drawn, the carbon nanotube film may be drawn in the same direction in a horizontal plane or may be drawn in a cross-shaped direction perpendicular to each other.
And s2, preparing the oriented carbon nanotube/graphene oxide composite membrane from the uniformly dispersed graphene oxide solution by a membrane forming technology.
In one embodiment, the dispersion of the graphene oxide solution may be ethanol, water or N, N-dimethylformamide.
In one embodiment, the concentration of the graphene oxide dispersion liquid may be 1-10mg/m L.
In one embodiment, the composite film forming technique may be vacuum filtration or spray coating.
The composite film can present different structural configurations when being formed, for example, a layer of carbon tube film is firstly drawn, and graphene oxide solution is filtered or sprayed to form a superposed composite film. On the basis, a carbon film can be drawn to form a sandwich-type composite film, or the operation can be repeated.
And s3, performing high-temperature graphitization treatment to obtain the high-crystallinity low-defect oriented carbon nanotube/graphene composite membrane.
The composite membrane is pretreated for 1-2 hours (h) at 800-1100 ℃, and then is graphitized for 0.5-2 hours at 1500-2850 ℃.
The existing preparation method of the graphene oxide is usually prepared by an oxidation method, the surface of the graphene oxide contains a large number of oxygen-containing functional groups, the impurity groups influence the crystallinity of the graphene oxide and generate phonon scattering in the heat transfer process, and the impurity groups have a side effect on heat conduction, so that the graphene oxide has a lower heat conductivity value, and the high-temperature thermal reduction method can effectively remove the oxygen-containing groups, thereby obviously improving the heat conduction performance of the composite film.
The technical solution of the present invention is further explained with reference to the drawings and the embodiments.
Comparative example 1
In the comparative example, a carbon nanotube/graphene oxide composite film without heat treatment was used as a comparison and was recorded as a sample at 25 ℃.
Comparative example 2
In the comparative example, a carbon nanotube/graphene oxide composite film which has not been subjected to high-temperature heat treatment is used as a comparison and is recorded as a 1000 ℃ sample.
Example 1
Will be plated with Fe/Al2O3/SiO2And (3) placing the silicon wafer of the catalyst layer in a horizontal tubular furnace, opening a gas source (argon, hydrogen and ethylene), ventilating argon to exhaust residual gas in the furnace chamber, stabilizing the flow of the argon gas to 700sccm, carrying out temperature programming on the furnace, wherein the flow of the hydrogen is 180sccm, starting an ethylene gas source (the flow: 200sccm) when the temperature is raised to 500 ℃, then carrying out temperature programming to 750 ℃ for 20min, reaching the growth time, ending the program, naturally cooling to room temperature, and taking out the spinnable carbon nanotube array sample.
Referring to fig. 3b, the spinnable carbon nanotube array is drawn into a cross-shaped carbon tube film in the horizontal plane by the surgical blade by using a drawing technique.
The preparation method of the high-crystallinity and low-defect oriented carbon nanotube/graphene composite membrane comprises the steps of dispersing graphene oxide in an ethanol solution, wherein the dispersion concentration of the graphene oxide can be controlled to be 2mg/m L, and carrying out suction filtration on a 10m L graphene oxide solution onto an oriented carbon tube membrane by taking a cross-shaped carbon tube membrane in a vacuum suction filtration mode to form the oriented carbon nanotube/graphene oxide composite membrane.
And placing the composite membrane in an argon atmosphere of a horizontal tube furnace, and carrying out pre-annealing treatment for 2 hours at 1000 ℃. And then placing the pretreated carbon composite membrane in a high-temperature graphitization furnace for graphitization treatment for 2h at the temperature of 1700 ℃ in an argon atmosphere to obtain the one-dimensional-two-dimensional orderly lapped carbon nanotube/graphene composite membrane.
Fig. 4a shows an XRD pattern of the carbon tube/graphene composite film after high temperature treatment, which indicates that the carbon tube/graphene oxide composite film is changed into a carbon tube/graphene composite film after high temperature treatment, and the high-crystallinity composite film is obtained after the high temperature treatment.
Fig. 4b shows a Raman chart of the carbon tube/graphene composite film after high temperature treatment, which shows that the defect degree of the composite film is obviously reduced after high temperature treatment.
Fig. 4c shows a graph of in-plane thermal diffusion coefficients of the carbon tube/graphene composite film after different high-temperature treatments, and tests show that the thermal conductivity of the composite film after the high-temperature graphitization treatment is greatly improved.
Example 2
Will be plated with Fe/Al2O3/SiO2And (3) placing the silicon wafer of the catalyst layer in a horizontal tubular furnace, opening a gas source (argon, hydrogen and ethylene), ventilating argon to exhaust residual gas in the furnace chamber, stabilizing the flow of the argon gas to 700sccm, carrying out temperature programming on the furnace, wherein the flow of the hydrogen is 180sccm, starting an ethylene gas source (the flow: 200sccm) when the temperature is raised to 500 ℃, then carrying out temperature programming to 750 ℃ for 20min, reaching the growth time, ending the program, naturally cooling to room temperature, and taking out the spinnable carbon nanotube array sample.
Referring to fig. 3(b), the spinnable carbon nanotube array is drawn into a cross-shaped carbon tube film in the horizontal plane by the surgical blade by using a drawing technique.
The preparation method of the high-crystallinity and low-defect oriented carbon nanotube/graphene composite membrane comprises the steps of dispersing graphene oxide in an ethanol solution, wherein the dispersion concentration of the graphene oxide can be controlled to be 2mg/m L, and carrying out suction filtration on a 10m L graphene oxide solution onto an oriented carbon tube membrane by taking a cross-shaped carbon tube membrane in a vacuum suction filtration mode to form the oriented carbon nanotube/graphene oxide composite membrane.
And placing the composite membrane in an argon atmosphere of a horizontal tube furnace, and carrying out pre-annealing treatment for 2 hours at 1000 ℃. And then placing the pretreated carbon composite membrane in a high-temperature graphitization furnace for graphitization treatment for 2h at 2300 ℃ under the argon atmosphere to obtain the one-dimensional-two-dimensional orderly lapped carbon nanotube/graphene composite membrane.
Fig. 4a shows an XRD pattern of the carbon tube/graphene composite film after high temperature treatment, which indicates that the carbon tube/graphene oxide composite film is changed into a carbon tube/graphene composite film after high temperature treatment, and the high-crystallinity composite film is obtained after the high temperature treatment.
Fig. 4b shows a Raman chart of the carbon tube/graphene composite film after high temperature treatment, which shows that the defect degree of the composite film is obviously reduced after high temperature treatment.
Fig. 4c shows a graph of in-plane thermal diffusion coefficients of the carbon tube/graphene composite film after different high-temperature treatments, and tests show that the thermal conductivity of the composite film after the high-temperature graphitization treatment is greatly improved.
Example 3
Will be plated with Fe/Al2O3/SiO2) The silicon chip of catalyst layer is placed in horizontal tubular furnace, opens the air supply (argon, hydrogen, ethylene), ventilates with argon and exhausts furnace chamber residual gas, stabilizes argon flow 700sccm, and stove program heating, hydrogen flow are 180sccm, opens ethylene air supply (flow) when rising to 500 degrees centigrade: 200sccm), then programming to 750 ℃ and maintaining for 20min, ending the program, naturally cooling to room temperature, and taking out the spinnable carbon nanotube array sample.
Referring to fig. 3(b), the spinnable carbon nanotube array is drawn into a cross-shaped carbon tube film in the horizontal plane by the surgical blade by using a drawing technique.
The preparation method of the high-crystallinity and low-defect oriented carbon nanotube/graphene composite membrane comprises the steps of dispersing graphene oxide in an ethanol solution, wherein the dispersion concentration of the graphene oxide can be controlled to be 2mg/m L, and carrying out suction filtration on a 10m L graphene oxide solution onto an oriented carbon tube membrane by taking a cross-shaped carbon tube membrane in a vacuum suction filtration mode to form the oriented carbon nanotube/graphene oxide composite membrane.
And placing the composite membrane in an argon atmosphere of a horizontal tube furnace, and carrying out pre-annealing treatment for 2 hours at 1000 ℃. And then placing the pretreated carbon composite membrane in a high-temperature graphitization furnace for graphitization treatment for 2h at the temperature of 2850 ℃ under the argon atmosphere to obtain the one-dimensional-two-dimensional orderly lapped carbon nanotube/graphene composite membrane.
Fig. 4a shows an XRD pattern of the carbon tube/graphene composite film after high temperature treatment, which indicates that the carbon tube/graphene oxide composite film is changed into a carbon tube/graphene composite film after high temperature treatment, and the high-crystallinity composite film is obtained after the high temperature treatment.
Fig. 4b shows a Raman chart of the carbon tube/graphene composite film after high temperature treatment, which shows that the defect degree of the composite film is obviously reduced after high temperature treatment.
Fig. 4c shows a graph of in-plane thermal diffusion coefficients of the carbon tube/graphene composite film after different high-temperature treatments, and tests show that the thermal conductivity of the composite film after the high-temperature graphitization treatment is greatly improved.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
Claims (10)
1. An oriented carbon nanotube/graphene composite heat-conducting film is characterized by comprising a carbon nanotube layer and a graphene layer compounded on the surface of the carbon nanotube layer,
the carbon nanotube layer is an oriented film.
2. The aligned carbon nanotube/graphene composite thermal conductive film according to claim 1, wherein the carbon nanotube layer is woven into a mesh shape by carbon nanotube wires.
3. The carbon nanotube/graphene composite thermal conductive film according to claim 1, wherein graphene layers are compounded on both surfaces of the carbon nanotube layer.
4. A semiconductor device using the aligned carbon nanotube/graphene composite thermal conductive film according to any one of claims 1 to 3 as a thermal interface material.
5. A preparation method of an oriented carbon nanotube/graphene composite heat conduction film is characterized by comprising the following steps:
s1, drawing the spinnable carbon nanotube array into an oriented film;
s2, compounding the graphene oxide solution on the surface of the orientation film;
and s3, carrying out heat treatment to obtain the composite heat conducting film.
6. The method of claim 5, wherein in step s1, the spinnable carbon nanotube array is fabricated by chemical vapor deposition.
7. The method for preparing an oriented carbon nanotube/graphene composite thermal conductive film according to claim 6, wherein the growth temperature is 700-840 ℃ and the heat preservation time is 10-60 minutes in the chemical vapor deposition process.
8. The method for preparing an oriented carbon nanotube/graphene composite thermal conductive film according to claim 5, wherein in step s2, the graphene oxide solution is compounded on the surface of the oriented film by vacuum filtration, spraying, screen printing, inkjet printing, roll coating or knife coating.
9. The method for preparing an oriented carbon nanotube/graphene composite thermal conductive film according to claim 5, wherein in the step s2, the concentration of the graphene oxide solution is 1-10mg/m L.
10. The method for preparing an aligned carbon nanotube/graphene composite thermal conductive film according to claim 5, wherein in step s3, the heat treatment process comprises:
pretreating at 800-;
heating to 1500 and 2850 ℃ for high-temperature treatment for 0.5-2 hours.
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| CN114206775A (en) * | 2020-12-28 | 2022-03-18 | 深圳烯湾科技有限公司 | Composite carbon nanotube film, preparation method thereof and layered heating device |
| WO2022140890A1 (en) * | 2020-12-28 | 2022-07-07 | 深圳烯湾科技有限公司 | Composite carbon nanotube film, preparation method therefor, and layered heating device |
| CN114538420A (en) * | 2022-01-25 | 2022-05-27 | 常州大学 | Preparation method of composite heat dissipation film material |
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