CN110581063A - Transfer method of graphene wafer - Google Patents
Transfer method of graphene wafer Download PDFInfo
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- CN110581063A CN110581063A CN201911005855.2A CN201911005855A CN110581063A CN 110581063 A CN110581063 A CN 110581063A CN 201911005855 A CN201911005855 A CN 201911005855A CN 110581063 A CN110581063 A CN 110581063A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
Abstract
The invention provides a transfer method of a graphene wafer, which comprises the following steps: forming a graphene wafer on a sapphire/metal substrate, wherein the sapphire/metal substrate is prepared through a magnetron sputtering process; and stripping the graphene wafer from the metal substrate by an electrochemical bubbling method. According to the method provided by the embodiment of the invention, the quality of the graphene growth substrate is improved, and the problem of damage of the graphene film transferred by the existing bubbling method is solved.
Description
Technical Field
The invention relates to a graphene wafer, in particular to a method for transferring the graphene wafer from a growth substrate.
Background
Due to good physicochemical properties of graphene, such as ultrahigh carrier mobility, high light transmittance, good mechanical properties and the like, the graphene is widely researched and shows potential practical values in the fields of transparent conductive films, photoelectric detection, catalysis, biological detection and the like.
Among the preparation methods of graphene, the chemical vapor deposition method for the surface of the copper foil has the advantages of high quality of the grown graphene, suitability for macro preparation and the like. However, it is often necessary to transfer the graphene films grown on copper foil and copper wafer substrates to a specific substrate for further applications. At present, the most common method for transferring graphene is an etching substrate transfer method, which uses etching liquid to etch away a copper substrate and leaves a complete graphene film.
In the past, an electrochemical bubbling method has been invented to strip a graphene film grown on a copper foil, but due to the quality problem of a copper foil substrate, the graphene film stripped by the bubbling method is usually seriously damaged, and is difficult to popularize in a large area.
Disclosure of Invention
One objective of the present invention is to provide a method for transferring a graphene wafer, including:
Forming a graphene wafer on a sapphire/metal substrate, wherein the sapphire/metal substrate is prepared through a magnetron sputtering process; and
And peeling the graphene wafer from the metal substrate by an electrochemical bubbling method.
According to an embodiment of the invention, the method comprises spin-coating a polymer on the graphene wafer as an auxiliary transfer medium, and peeling the polymer/graphene wafer from the metal substrate by an electrochemical bubbling method.
According to an embodiment of the invention, the polymer comprises PMMA and/or PDMS, and the rotation speed of spin coating the polymer is 200-6000 rpm.
According to an embodiment of the present invention, the method includes transferring the exfoliated polymer/graphene wafer onto a target substrate.
According to an embodiment of the invention, the target substrate is sapphire or Si/SiO2A substrate.
According to an embodiment of the present invention, the polymer is removed from the graphene wafer using acetone.
According to an embodiment of the invention, the polymer/graphene wafer is transferred to a target substrate by a fishing device.
According to an embodiment of the invention, the fishing device comprises a fishing part and a holding part, wherein the fishing part is provided with a plane for bearing the graphene wafer.
According to an embodiment of the present invention, the electrochemical bubbling method uses a sodium hydroxide solution as a bubbling solution, an applied voltage is 1 to 10V, and a concentration of the sodium hydroxide solution is 0.01 to 10 mol/L.
according to an embodiment of the invention, the metal substrate is copper.
According to the method provided by the embodiment of the invention, the quality of the graphene growth substrate is improved, and the problem of damage of the graphene film transferred by the existing bubbling method is solved.
Drawings
Fig. 1 is a schematic structural view of a bubbling device according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a fishing device according to an embodiment of the present invention;
Fig. 3a is a photograph of a graphene film/copper/sapphire wafer prepared in example 1 of the present invention;
fig. 3b is an optical microscope picture of the graphene film/copper/sapphire wafer prepared in example 1 of the present invention;
Fig. 3c is a scanning electron microscope picture of the graphene film/copper/sapphire wafer prepared in example 1 of the present invention;
Fig. 3d is an atomic force microscope picture of the graphene film/copper/sapphire wafer prepared in example 1 of the present invention;
Fig. 3e is a raman spectrum of the graphene film/copper/sapphire wafer prepared in example 1 of the present invention;
FIG. 3f shows the transferred graphene film/Si/SiO in example 1 of the present invention2A photograph of the substrate.
FIG. 3g shows the transferred graphene film/Si/SiO in example 1 of the present invention2Base optical microscope pictures.
FIG. 3h shows the transferred graphene film/Si/SiO in example 1 of the present invention2Raman spectroscopy of the substrate.
FIG. 4 shows a single crystal Cu-Ni alloy wafer obtained in example 2 of the present invention.
Detailed Description
Exemplary embodiments that embody features and advantages of the invention are described in detail below in the specification. It is to be understood that the invention is capable of other embodiments and that various changes in form and details may be made therein without departing from the scope of the invention and the description and drawings are to be regarded as illustrative in nature and not as restrictive.
An embodiment of the present invention provides a graphene wafer transfer method, including:
forming a graphene wafer on a sapphire/metal substrate, wherein the sapphire/metal substrate is prepared through a magnetron sputtering process; and
And stripping the graphene wafer from the metal substrate by an electrochemical bubbling method.
In one embodiment, a metal substrate may be formed on a sapphire wafer by a magnetron sputtering process.
According to the method provided by the embodiment of the invention, the quality of the graphene growth substrate is improved by using the sapphire/metal substrate, and the problem of damage of the graphene film transferred by the existing bubbling method (taking a metal foil as a transfer substrate) is solved.
in one embodiment, the factors affecting the quality of the substrate are mainly flatness, defects, wrinkles, grain boundaries, particles, and the like.
According to the method provided by the embodiment of the invention, the graphene wafer is transferred by the electrochemical bubbling method, compared with the traditional etching method, the transfer time is changed from hours to minutes, and the transfer rate of the single crystal graphene wafer is greatly improved.
In one embodiment, the sapphire/metal substrate being peeled can be recycled more than three times and has a high quality.
according to the method provided by the embodiment of the invention, the stripped sapphire/metal substrate can be recycled, so that the production cost is reduced.
In one embodiment, the metal substrate may be copper, copper-nickel alloy, or other metal.
In one embodiment, a graphene wafer may be epitaxially grown on a metal of a sapphire/metal substrate by a chemical vapor deposition process.
In one embodiment, a polymer is spin-coated on a graphene wafer as an auxiliary transfer medium, and the polymer/graphene wafer is peeled off from the metal substrate by an electrochemical bubbling method.
In one embodiment, the polymer used as the auxiliary transfer medium may be PMMA (polymethyl methacrylate), PDMS (polydimethylsiloxane), or the like.
in one embodiment, the thickness of the polymer layer formed on the graphene wafer may be varied by controlling the rotation speed of the spin-on polymer.
In one embodiment, the spin coating of the polymer may be performed at a speed of 200 to 6000rpm, such as 300rpm, 500rpm, 1000rpm, 1500rpm, 2000rpm, 2500rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm, 5000rpm, 5500rpm, and the like.
In one embodiment, the electrochemical bubbling method uses a sodium hydroxide solution as a bubbling solution, and the concentration of the sodium hydroxide solution may be 0.01 to 10mol/L, for example, 0.1mol/L, 0.2mol/L, 0.5mol/L, 1mol/L, 2mol/L, 5mol/L, 8mol/L, and the like.
In one embodiment, the applied voltage used in the electrochemical bubbling method is 1 to 10V, such as 2V, 3V, 5V, 6V, 8V, etc.
the transfer method of the graphene wafer according to an embodiment of the present invention includes:
(1) Epitaxially growing a single crystal copper substrate on the single crystal sapphire wafer by adopting a magnetron sputtering method to obtain a sapphire wafer/single crystal copper substrate;
(2) Preparing a single crystal graphene wafer on a copper layer of a sapphire wafer/single crystal copper substrate by a chemical vapor deposition method;
(3) Spin-coating a polymer with a certain thickness on the obtained single crystal graphene wafer to serve as an auxiliary transfer medium;
(4) Stripping the polymer/graphene film from the copper substrate by adopting an electrochemical bubbling method;
(5) Transferring the polymer/graphene film to a target substrate;
(6) The polymer transfer medium is removed with a solvent.
in one embodiment, the target substrate may be sapphire or Si/SiO2A substrate.
in one embodiment, the solvent used to remove the polymer transfer medium may be acetone.
In one embodiment, an electrochemical bubbling process is performed by the bubbling device shown in fig. 1, the device includes a slide rail 2, a wafer carrier 4 and a bubbling tank 5, a bubbling solution is disposed in the bubbling tank 5, a wafer 3 including sapphire, a metal substrate, and a graphene film-polymer is disposed on the wafer carrier 4 and enters the bubbling tank 5 through the slide rail 2, wherein the wafer 3 is used as a cathode, a copper plate is used as an anode for electrochemical bubbling, after the graphene-polymer is peeled off from the metal substrate, the graphene-polymer can be fished out from the bubbling tank 5 by using a fishing device shown in fig. 2, and the graphene film-polymer can be further transferred to a target substrate by using the fishing device.
In one embodiment, the anode of the electrochemical bubbling process can be a copper plate or a graphite plate.
in one embodiment, the wafer 3 is connected to a power source through the cathode electrode clamp 6, and the anode is connected to the power source through the anode electrode clamp 1.
As shown in fig. 2, the fishing device according to an embodiment of the present invention includes a fishing portion 10 for receiving a graphene film to be fished, and a holding portion 20, wherein the fishing portion 10 has a plane 11 for carrying the graphene film.
In one embodiment, the plane 11 of the fishing part 10 is rectangular, a blocking wall 12 perpendicular to the plane 11 is disposed along three sides of the plane 11, and the other side is an opening for facilitating the entry of the graphene film.
In one embodiment, the holding portion 20 is disposed on the fishing portion 10, the holding portion 20 may be a vertical rod perpendicular to the plane 11 of the fishing portion 10, and the number of the vertical rods may be two.
In one embodiment, when the fishing tool is used, the grip 20 is held by hand to immerse the fishing part 10 below the liquid surface so that the graphene film floating on the liquid surface is positioned above the fishing part 10, and the fishing part 10 is gradually raised until the graphene film is laid on the plane 11 of the fishing part 10.
according to the embodiment of the invention, the single crystal graphene wafer prepared by the CVD method is transferred from the growth substrate to the target substrate by adopting the electrochemical bubbling method, and the method has a very good effect particularly on the transfer of the single crystal graphene grown on the hard substrate. Compared with the traditional bubbling method, the method has the advantages of less bubbles, smoother graphene, less damage and defects, simpler operation and obvious advantages, so that the graphene single crystal wafer prepared by epitaxial growth of the copper/sapphire single crystal has very wide application prospects in the fields of communication, electronics, graphene preparation and the like.
According to the graphene wafer transfer method provided by the embodiment of the invention, the metal substrate is formed on the sapphire wafer through the magnetron sputtering process, and the graphene film is epitaxially grown, so that the surface of the prepared single crystal graphene wafer is flat enough and free of defects, the damage of the graphene film in the transfer process is greatly reduced, and the quality of the obtained graphene film is improved.
According to the transfer method of the graphene wafer, bubbles remained in the graphene film-polymer can be removed through the use of the fishing device, so that the obtained film is flat and free of bubbles.
The following further describes a graphene wafer transfer method according to an embodiment of the invention with reference to the accompanying drawings and specific examples. Wherein, the raw materials are all obtained from the market.
EXAMPLE 14 bubbling transfer of Single Crystal graphene wafers on a Cu/sapphire Single Crystal substrate
Step (1): single crystal copper was prepared according to the method disclosed in patent application No. 201710522321.1, resulting in a 500nm thick copper (111) single crystal on a 4 inch sapphire single crystal substrate;
The growth conditions for graphene are similar to those of the patent application No. 201710523050.1, in brief, copper (111) single crystal thin film/sapphire is first grown at a carrier gas flow of 2000sccm Ar and 40sccm H2the temperature of the gas is raised from room temperature to 1000 ℃ for 1 hour, and 40sccm of diluted methane is introduced, wherein the volume percentage of methane in the diluted carbon source gas is 0.1%. After 120 minutes of growth, the entire wafer surface can be grown, and the resulting product is shown in fig. 3a, the optical microscope picture is shown in fig. 3b, the scanning electron microscope picture is shown in fig. 3c, the atomic force microscope is shown in fig. 3d, and the raman spectrum is shown in fig. 3 e. Graphene overgrowth can be seen, with good uniformity.
step (2): and transferring the prepared graphene film/growth substrate, and coating a layer of PMMA film on the surface of the graphene film by using a spin coater, wherein the rotating speed of the spin coater is 1000 revolutions per minute, and the spin coating time is 60 seconds. The resulting substrate was baked on a hot stage at 100 ℃ for 3 minutes to cure.
And (3): 0.2mol/L NaOH aqueous solution is prepared as a bubbling solution. Connecting an external power supply, keeping the voltage at 3V, keeping the current less than 0.1A in the bubbling process, placing the PMMA/graphene/growth substrate on the bubbling device shown in the figure 1, taking the PMMA/graphene/growth substrate as a cathode, taking a copper plate as an anode, and carrying the substrate by the bubbling device to slowly enter the solution. The PMMA/graphene film entering the NaOH solution part is stripped from the substrate due to micro bubbles generated by the cathode and floats above the liquid level; and continuously and slowly putting the materials in the reactor, and always keeping the PMMA/graphene film floating above the liquid level until the PMMA/graphene film is completely stripped.
And (4): fishing out the PMMA/graphene film by using the fishing device of FIG. 2, putting the PMMA/graphene film on the surface of pure water, standing and floating, repeatedly fishing out the PMMA/graphene film from the pure water, putting new pure water, floating on the surface, repeating for several times until bubbles disappear, and standing for 1 h. With a target substrate(by Si/SiO)2base) and taking out, standing and drying. And after sufficient drying, removing the PMMA with hot acetone to obtain a wrinkle-free, clean and complete graphene film/target substrate, as shown in fig. 3 f. The optical microscope image of the transferred graphene film is shown in fig. 3g, and the raman spectrum is shown in fig. 3h, so that the transferred film is complete and no new defect is introduced.
Example two-phase solution bubble transfer of graphene on a 24 inch CuNi/sapphire single crystal substrate
step (1): the single crystal copper nickel was prepared according to the method disclosed in patent application No. 201810253431.7, and a CuNi (111) single crystal was obtained on a 4-inch sapphire single crystal substrate to a thickness of 500 nm;
The growth conditions for graphene are similar to those of the patent application No. 201710523050.1, in brief, CuNi (111) single crystal thin film/sapphire is first grown at a carrier gas flow of 2000sccm Ar and 40sccm H2the temperature of the gas is raised from room temperature to 1000 ℃ for 1 hour, and 40sccm of diluted methane is introduced, wherein the volume percentage of methane in the diluted carbon source gas is 0.1%. After the growth is carried out for 10 minutes, the whole wafer surface can be grown, and the obtained product is shown in fig. 4, and the graphene can be detected to be grown and has good uniformity.
Step (2): the prepared graphene film/growth substrate is transferred in the same manner as the step (2) of the embodiment 1, and a layer of PMMA film is coated on the surface of the graphene film by a spin coater, wherein the rotating speed of the spin coater is 1000 revolutions per minute, and the spin coating time is 60 seconds. The resulting substrate was baked on a hot stage at 100 ℃ for 3 minutes to cure.
And (3): in the same manner as in step (3) of example 1, a 0.2mol/L aqueous NaOH solution was prepared as a bubbling solution. Connecting an external power supply, keeping the voltage at 3V, keeping the current less than 0.1A in the bubbling process, placing the PMMA/graphene/growth substrate on the bubbling device shown in the figure 1, taking the PMMA/graphene/growth substrate as a cathode, and carrying the substrate by the bubbling device to slowly enter the solution. The PMMA/graphene film entering the NaOH solution part is stripped from the substrate due to micro bubbles generated by the cathode and floats above the liquid level; and continuously and slowly putting the materials in the reactor, and always keeping the PMMA/graphene film floating above the liquid level until the PMMA/graphene film is completely stripped.
And (4): in the same manner as in the step (4) of example 1, the part of the bubbling solution was placed in the fishing device shown in fig. 2, so as to avoid contamination due to the auxiliary solution, the PMMA/graphene film was fished out, placed on the surface of pure water and left to float, the fishing out from the pure water was repeated, a new pure water was placed on the surface and floated, and the process was repeated several times until the bubbles disappeared and left to stand for 1 hour. With a target substrate (Si/SiO)2base) and taking out, standing and drying. And after full drying, removing PMMA by using hot acetone to obtain a clean and complete graphene film/target substrate without folds. The integrity of the transferred film can be known through detection, and no new defects are introduced.
Unless otherwise defined, all terms used herein have the meanings commonly understood by those skilled in the art.
The described embodiments of the present invention are for illustrative purposes only and are not intended to limit the scope of the present invention, and those skilled in the art may make various other substitutions, alterations, and modifications within the scope of the present invention, and thus, the present invention is not limited to the above-described embodiments but only by the claims.
Claims (10)
1. A graphene wafer transfer method comprises the following steps:
Forming a graphene wafer on a sapphire/metal substrate, wherein the sapphire/metal substrate is prepared through a magnetron sputtering process; and
And peeling the graphene wafer from the metal substrate by an electrochemical bubbling method.
2. The method of claim 1, comprising spin coating a polymer on the graphene wafer as an auxiliary transfer medium, and peeling the polymer/graphene wafer from the metal substrate by an electrochemical bubbling method.
3. The method of claim 2, wherein the polymer comprises PMMA and/or PDMS, and the polymer is spin coated at a speed of 200-6000 rpm.
4. the method of claim 2, comprising transferring the exfoliated polymer/graphene wafer onto a target substrate.
5. The method of claim 4, wherein the target substrate is sapphire or Si/SiO2A substrate.
6. The method of claim 4, wherein the polymer is removed from the graphene wafer using acetone.
7. the method of claim 2, wherein the polymer/graphene wafer is transferred to a target substrate by a fishing device.
8. the method of claim 7, wherein the fishing device comprises a fishing portion and a holding portion, and the fishing portion has a plane to carry the graphene wafer.
9. The method according to claim 1, wherein the electrochemical bubbling method uses a sodium hydroxide solution as a bubbling solution, an applied voltage is 1-10V, and the concentration of the sodium hydroxide solution is 0.01-10 mol/L.
10. The method of claim 1, wherein the metal substrate is copper.
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Cited By (2)
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| CN111232964A (en) * | 2020-01-19 | 2020-06-05 | 北京石墨烯研究院 | Graphene wafer transfer method, graphene wafer and bubbling system |
| CN114956062A (en) * | 2021-02-25 | 2022-08-30 | 北京石墨烯研究院 | Transfer method of single crystal wafer graphene film |
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Application publication date: 20191217 |